 
data_s92
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C36 H76 Co2 O18 P6 Zr'
_chemical_formula_sum
 'C36 H76 Co2 O18 P6 Zr'
_chemical_formula_weight          1191.87
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P'  'P'   0.1023   0.0942
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Co'  'Co'   0.3494   0.9721
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zr'  'Zr'  -2.9673   0.5597
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            Triclinic
_symmetry_space_group_name_H-M    P-1
_symmetry_space_group_name_hall   '-P 1'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    12.353(3)
_cell_length_b                    12.392(4)
_cell_length_c                    18.1099(16)
_cell_angle_alpha                 83.286(14)
_cell_angle_beta                  82.649(14)
_cell_angle_gamma                 74.120(12)
_cell_volume                      2634.7(11)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        unk
_exptl_crystal_colour             unk
_exptl_crystal_size_max           0.24
_exptl_crystal_size_mid           0.11
_exptl_crystal_size_min           0.11
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.502
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1240
_exptl_absorpt_coefficient_mu     1.062
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.7846
_exptl_absorpt_correction_T_max   0.8921
_exptl_absorpt_process_details    'SORTAV (R.H.Blessing, 1995, 1997)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71069
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source         'rotating anode generator'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Delft instruments FAST area detector'
_diffrn_measurement_method
 'Intensity measurements as described by Darr, Drake, Hursthouse & Malik (1993)'
_diffrn_standards_number         'None'
_diffrn_standards_interval_count 'N/A'
_diffrn_standards_interval_time  'N/A'
_diffrn_standards_decay_%        'N/A'
_diffrn_reflns_number             10889
_diffrn_reflns_av_R_equivalents   0.0900
_diffrn_reflns_av_sigmaI/netI     0.2826
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_l_min        -20
_diffrn_reflns_limit_l_max        20
_diffrn_reflns_theta_min          1.97
_diffrn_reflns_theta_max          25.13
_reflns_number_total              7115
_reflns_number_gt                 3816
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection        'MADNES (Pflugrath & Messerschmidt, 1989)'
_computing_cell_refinement        REFINE
_computing_data_reduction         'ABSURD (Karaulov, 1992)'
_computing_structure_solution     'SIR92 (Altomare, Cascarano, Giacovazzo & Guaglitardi, 1993)'
_computing_structure_refinement   'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material   SHELXL97
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          7115
_refine_ls_number_parameters      571
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1038
_refine_ls_R_factor_gt            0.0570
_refine_ls_wR_factor_ref          0.1201
_refine_ls_wR_factor_gt           0.1094
_refine_ls_goodness_of_fit_ref    0.749
_refine_ls_restrained_S_all       0.749
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Zr1 Zr 0.0000 0.0000 0.5000 0.0200(2) Uani 1 2 d S . .
Zr2 Zr 0.5000 0.5000 0.0000 0.0226(2) Uani 1 2 d S . .
Co1 Co 0.14787(7) 0.24359(6) 0.49826(4) 0.0215(2) Uani 1 1 d . . .
Co2 Co 0.79929(7) 0.34020(7) 0.06126(5) 0.0276(2) Uani 1 1 d . . .
P1 P 0.02610(14) 0.21060(13) 0.58851(9) 0.0222(4) Uani 1 1 d . . .
P2 P 0.24228(14) 0.06971(13) 0.49504(9) 0.0214(4) Uani 1 1 d . . .
P3 P 0.03903(14) 0.24148(13) 0.41515(9) 0.0215(4) Uani 1 1 d . . .
P4 P 0.69541(16) 0.25679(15) 0.01531(10) 0.0378(5) Uani 1 1 d . . .
P5 P 0.33353(16) 0.56860(15) -0.13616(10) 0.0329(5) Uani 1 1 d . . .
P6 P 0.22890(16) 0.51553(16) 0.02153(10) 0.0349(5) Uani 1 1 d . . .
O1 O -0.0163(3) 0.1051(3) 0.5837(2) 0.0234(11) Uani 1 1 d . . .
O2 O 0.1713(3) -0.0151(3) 0.4899(2) 0.0239(11) Uani 1 1 d . . .
O3 O -0.0175(3) 0.1422(3) 0.4242(2) 0.0210(10) Uani 1 1 d . . .
O4 O 0.0817(3) 0.1922(3) 0.6661(2) 0.0272(11) Uani 1 1 d . . .
O5 O -0.0869(3) 0.3065(3) 0.6100(2) 0.0331(12) Uani 1 1 d . . .
O6 O 0.3378(3) 0.0480(3) 0.4258(2) 0.0278(12) Uani 1 1 d . . .
O7 O 0.3168(4) 0.0181(3) 0.5644(2) 0.0357(13) Uani 1 1 d . B .
O8 O -0.0606(3) 0.3524(3) 0.4056(2) 0.0281(12) Uani 1 1 d . . .
O9 O 0.0969(4) 0.2428(3) 0.3312(2) 0.0340(12) Uani 1 1 d . . .
O10 O 0.5706(4) 0.3276(3) 0.0117(2) 0.0364(13) Uani 1 1 d . . .
O11 O 0.4375(4) 0.4895(3) -0.0992(2) 0.0331(12) Uani 1 1 d . . .
O12 O 0.3468(3) 0.4846(4) 0.0539(2) 0.0354(13) Uani 1 1 d . . .
O13 O 0.7395(4) 0.2213(4) -0.0678(2) 0.0409(13) Uani 1 1 d . . .
O14 O 0.6849(4) 0.1331(4) 0.0520(3) 0.0606(17) Uani 1 1 d . . .
O15 O 0.3849(4) 0.6528(4) -0.1984(2) 0.0396(14) Uani 1 1 d . . .
O16 O 0.3013(4) 0.4924(4) -0.1923(2) 0.0433(14) Uani 1 1 d . . .
O17 O 0.2170(4) 0.4036(3) -0.0090(2) 0.0380(13) Uani 1 1 d . . .
O18 O 0.1383(4) 0.5214(4) 0.0937(2) 0.0418(14) Uani 1 1 d . . .
C1 C 0.2588(5) 0.2921(5) 0.5558(3) 0.0309(18) Uani 1 1 d . . .
H1 H 0.2663 0.2449 0.6011 0.037 Uiso 1 1 calc R . .
C2 C 0.1652(5) 0.3798(5) 0.5404(3) 0.0271(18) Uani 1 1 d . . .
H2 H 0.1112 0.4207 0.5762 0.033 Uiso 1 1 calc R . .
C3 C 0.1644(5) 0.3974(5) 0.4629(4) 0.0315(18) Uani 1 1 d . . .
H3 H 0.1097 0.4511 0.4358 0.038 Uiso 1 1 calc R . .
C4 C 0.2586(6) 0.3212(5) 0.4338(4) 0.0322(18) Uani 1 1 d . . .
H4 H 0.2675 0.2956 0.3854 0.039 Uiso 1 1 calc R . .
C5 C 0.3470(6) 0.2832(5) 0.4894(4) 0.038(2) Uani 1 1 d . . .
H5 H 0.3904 0.2030 0.4844 0.045 Uiso 1 1 calc R . .
C6 C 0.4286(5) 0.3597(5) 0.4870(4) 0.042(2) Uani 1 1 d . . .
H6A H 0.4783 0.3532 0.4401 0.063 Uiso 1 1 calc R . .
H6B H 0.4745 0.3360 0.5292 0.063 Uiso 1 1 calc R . .
H6C H 0.3845 0.4382 0.4901 0.063 Uiso 1 1 calc R . .
C7 C 0.0206(6) 0.1592(6) 0.7335(3) 0.042(2) Uani 1 1 d . . .
H7A H 0.0054 0.0858 0.7296 0.051 Uiso 1 1 calc R . .
H7B H -0.0527 0.2159 0.7424 0.051 Uiso 1 1 calc R . .
C8 C 0.0919(6) 0.1500(6) 0.7976(3) 0.049(2) Uani 1 1 d . . .
H8A H 0.0560 0.1182 0.8433 0.074 Uiso 1 1 calc R . .
H8B H 0.0981 0.2249 0.8054 0.074 Uiso 1 1 calc R . .
H8C H 0.1676 0.1008 0.7855 0.074 Uiso 1 1 calc R . .
C9 C -0.1911(6) 0.3222(5) 0.5768(4) 0.039(2) Uani 1 1 d . . .
H9A H -0.1947 0.2504 0.5597 0.047 Uiso 1 1 calc R . .
H9B H -0.1949 0.3787 0.5331 0.047 Uiso 1 1 calc R . .
C10 C -0.2861(7) 0.3611(8) 0.6335(5) 0.100(4) Uani 1 1 d . . .
H10A H -0.2983 0.2966 0.6671 0.150 Uiso 1 1 calc R . .
H10B H -0.3547 0.3973 0.6089 0.150 Uiso 1 1 calc R . .
H10C H -0.2687 0.4154 0.6624 0.150 Uiso 1 1 calc R . .
C11 C 0.4111(6) -0.0599(5) 0.4163(4) 0.045(2) Uani 1 1 d . . .
H11A H 0.3708 -0.1176 0.4367 0.054 Uiso 1 1 calc R . .
H11B H 0.4767 -0.0706 0.4451 0.054 Uiso 1 1 calc R . .
C12 C 0.4504(10) -0.0759(8) 0.3405(5) 0.169(6) Uani 1 1 d . . .
H12A H 0.3944 -0.0281 0.3086 0.254 Uiso 1 1 calc R . .
H12B H 0.4616 -0.1550 0.3320 0.254 Uiso 1 1 calc R . .
H12C H 0.5223 -0.0555 0.3284 0.254 Uiso 1 1 calc R . .
C13 C 0.3135(10) -0.0729(9) 0.6101(6) 0.169(5) Uani 1 1 d . . .
H13A H 0.2661 -0.1061 0.5842 0.203 Uiso 1 1 calc R A 1
H13B H 0.3913 -0.1206 0.5994 0.203 Uiso 1 1 calc R A 1
C14 C 0.2922(16) -0.1057(10) 0.6731(6) 0.282(11) Uani 1 1 d . B 1
H14A H 0.2534 -0.1651 0.6744 0.424 Uiso 1 1 calc R B 1
H14B H 0.2431 -0.0432 0.7000 0.424 Uiso 1 1 calc R B 1
H14C H 0.3625 -0.1357 0.6969 0.424 Uiso 1 1 calc R B 1
C15 C -0.1337(6) 0.3660(6) 0.3469(4) 0.040(2) Uani 1 1 d . . .
H15A H -0.1146 0.2961 0.3211 0.048 Uiso 1 1 calc R . .
H15B H -0.1225 0.4283 0.3098 0.048 Uiso 1 1 calc R . .
C16 C -0.2560(6) 0.3916(7) 0.3805(4) 0.059(2) Uani 1 1 d . . .
H16A H -0.3059 0.4112 0.3404 0.088 Uiso 1 1 calc R . .
H16B H -0.2716 0.4550 0.4115 0.088 Uiso 1 1 calc R . .
H16C H -0.2693 0.3252 0.4114 0.088 Uiso 1 1 calc R . .
C17 C 0.1458(8) 0.1389(7) 0.2954(4) 0.074(3) Uani 1 1 d . . .
H17A H 0.1849 0.0801 0.3321 0.088 Uiso 1 1 calc R . .
H17B H 0.0847 0.1128 0.2788 0.088 Uiso 1 1 calc R . .
C18 C 0.2219(8) 0.1538(7) 0.2348(5) 0.091(4) Uani 1 1 d . . .
H18A H 0.2541 0.0823 0.2122 0.137 Uiso 1 1 calc R . .
H18B H 0.2827 0.1791 0.2513 0.137 Uiso 1 1 calc R . .
H18C H 0.1830 0.2105 0.1978 0.137 Uiso 1 1 calc R . .
C19 C 0.8849(6) 0.2109(6) 0.1325(4) 0.043(2) Uani 1 1 d . . .
H19 H 0.8311 0.1888 0.1692 0.051 Uiso 1 1 calc R . .
C20 C 0.9200(6) 0.3100(6) 0.1293(4) 0.036(2) Uani 1 1 d . . .
H20 H 0.9143 0.3541 0.1699 0.043 Uiso 1 1 calc R . .
C21 C 0.9636(6) 0.3322(6) 0.0579(4) 0.041(2) Uani 1 1 d . . .
H21 H 0.9942 0.3941 0.0404 0.049 Uiso 1 1 calc R . .
C22 C 0.9560(6) 0.2500(6) 0.0155(4) 0.050(2) Uani 1 1 d . . .
H22 H 0.9573 0.2552 -0.0374 0.059 Uiso 1 1 calc R . .
C23 C 0.9450(7) 0.1477(6) 0.0702(4) 0.055(2) Uani 1 1 d . . .
H23 H 0.8970 0.1056 0.0516 0.066 Uiso 1 1 calc R . .
C24 C 1.0656(7) 0.0691(6) 0.0828(5) 0.070(3) Uani 1 1 d . . .
H24A H 1.1081 0.0506 0.0344 0.105 Uiso 1 1 calc R . .
H24B H 1.0581 -0.0004 0.1125 0.105 Uiso 1 1 calc R . .
H24C H 1.1060 0.1079 0.1095 0.105 Uiso 1 1 calc R . .
C25 C 0.6711(8) 0.1779(9) -0.1075(5) 0.100(4) Uani 1 1 d . . .
H25A H 0.6984 0.0947 -0.1015 0.120 Uiso 1 1 calc R . .
H25B H 0.5933 0.1981 -0.0820 0.120 Uiso 1 1 calc R . .
C26 C 0.6643(12) 0.2057(14) -0.1747(7) 0.242(9) Uani 1 1 d . . .
H26A H 0.5968 0.1902 -0.1894 0.363 Uiso 1 1 calc R . .
H26B H 0.7317 0.1627 -0.2035 0.363 Uiso 1 1 calc R . .
H26C H 0.6590 0.2863 -0.1846 0.363 Uiso 1 1 calc R . .
C27 C 0.6237(8) 0.1186(8) 0.1210(5) 0.098(4) Uani 1 1 d . . .
H27A H 0.5632 0.1885 0.1295 0.118 Uiso 1 1 calc R . .
H27B H 0.6747 0.1061 0.1609 0.118 Uiso 1 1 calc R . .
C28 C 0.5749(9) 0.0284(8) 0.1260(6) 0.143(4) Uani 1 1 d . . .
H28A H 0.5197 0.0323 0.1703 0.215 Uiso 1 1 calc R . .
H28B H 0.6340 -0.0426 0.1302 0.215 Uiso 1 1 calc R . .
H28C H 0.5368 0.0322 0.0812 0.215 Uiso 1 1 calc R . .
C29 C 0.4815(7) 0.6106(7) -0.2438(4) 0.065(3) Uani 1 1 d . . .
H29A H 0.4650 0.6277 -0.2966 0.078 Uiso 1 1 calc R . .
H29B H 0.5052 0.5276 -0.2337 0.078 Uiso 1 1 calc R . .
C30 C 0.5750(8) 0.6570(8) -0.2329(4) 0.085(3) Uani 1 1 d . . .
H30A H 0.6447 0.6159 -0.2605 0.128 Uiso 1 1 calc R . .
H30B H 0.5851 0.6493 -0.1795 0.128 Uiso 1 1 calc R . .
H30C H 0.5575 0.7368 -0.2513 0.128 Uiso 1 1 calc R . .
C31 C 0.3123(9) 0.3816(7) -0.1831(5) 0.106(4) Uani 1 1 d . . .
H31A H 0.2467 0.3681 -0.1495 0.127 Uiso 1 1 calc R . .
H31B H 0.3809 0.3458 -0.1573 0.127 Uiso 1 1 calc R . .
C32 C 0.3201(8) 0.3278(6) -0.2468(4) 0.089(3) Uani 1 1 d . . .
H32A H 0.3159 0.2501 -0.2329 0.134 Uiso 1 1 calc R . .
H32B H 0.3922 0.3275 -0.2765 0.134 Uiso 1 1 calc R . .
H32C H 0.2575 0.3676 -0.2763 0.134 Uiso 1 1 calc R . .
C33 C 0.2511(7) 0.2949(6) 0.0375(4) 0.057(2) Uani 1 1 d . . .
H33A H 0.3105 0.2978 0.0685 0.068 Uiso 1 1 calc R . .
H33B H 0.1852 0.2829 0.0715 0.068 Uiso 1 1 calc R . .
C34 C 0.2942(9) 0.2004(6) -0.0101(5) 0.097(4) Uani 1 1 d . . .
H34A H 0.3674 0.2047 -0.0368 0.146 Uiso 1 1 calc R . .
H34B H 0.2403 0.2049 -0.0464 0.146 Uiso 1 1 calc R . .
H34C H 0.3036 0.1290 0.0211 0.146 Uiso 1 1 calc R . .
C35 C 0.1436(6) 0.5725(7) 0.1569(4) 0.062(3) Uani 1 1 d . . .
H35A H 0.1152 0.6553 0.1478 0.075 Uiso 1 1 calc R . .
H35B H 0.2228 0.5548 0.1689 0.075 Uiso 1 1 calc R . .
C36 C 0.0717(7) 0.5293(6) 0.2211(4) 0.063(3) Uani 1 1 d . . .
H36A H 0.0758 0.5635 0.2664 0.094 Uiso 1 1 calc R . .
H36B H 0.0997 0.4472 0.2292 0.094 Uiso 1 1 calc R . .
H36C H -0.0070 0.5490 0.2093 0.094 Uiso 1 1 calc R . .
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Zr1 O2 2.059(4) . ?
Zr1 O2 2.059(4) 2_556 ?
Zr1 O1 2.067(3) . ?
Zr1 O1 2.067(3) 2_556 ?
Zr1 O3 2.083(4) . ?
Zr1 O3 2.083(4) 2_556 ?
Zr2 O12 2.062(4) . ?
Zr2 O12 2.062(4) 2_665 ?
Zr2 O10 2.071(4) . ?
Zr2 O10 2.071(4) 2_665 ?
Zr2 O11 2.075(4) 2_665 ?
Zr2 O11 2.075(4) . ?
Co1 C3 1.994(6) . ?
Co1 C2 2.005(6) . ?
Co1 C4 2.051(7) . ?
Co1 C1 2.070(6) . ?
Co1 P3 2.1494(18) . ?
Co1 P2 2.1548(18) . ?
Co1 P1 2.1569(19) . ?
Co2 C20 1.984(6) . ?
Co2 C21 1.999(7) . ?
Co2 C19 2.071(7) . ?
Co2 C22 2.075(7) . ?
Co2 P5 2.141(2) 2_665 ?
Co2 P4 2.147(2) . ?
Co2 P6 2.175(2) 2_665 ?
P1 O1 1.550(4) . ?
P1 O5 1.604(4) . ?
P1 O4 1.607(4) . ?
P2 O2 1.558(4) . ?
P2 O6 1.601(4) . ?
P2 O7 1.619(4) . ?
P3 O3 1.556(4) . ?
P3 O8 1.583(4) . ?
P3 O9 1.595(4) . ?
P4 O10 1.557(4) . ?
P4 O13 1.603(4) . ?
P4 O14 1.630(5) . ?
P5 O11 1.561(4) . ?
P5 O16 1.618(4) . ?
P5 O15 1.633(5) . ?
P5 Co2 2.141(2) 2_665 ?
P6 O12 1.572(4) . ?
P6 O17 1.601(4) . ?
P6 O18 1.603(4) . ?
P6 Co2 2.175(2) 2_665 ?
O4 C7 1.430(7) . ?
O5 C9 1.445(8) . ?
O6 C11 1.410(7) . ?
O7 C13 1.325(10) . ?
O8 C15 1.447(7) . ?
O9 C17 1.454(8) . ?
O13 C25 1.420(9) . ?
O14 C27 1.394(9) . ?
O15 C29 1.372(8) . ?
O16 C31 1.335(9) . ?
O17 C33 1.489(8) . ?
O18 C35 1.387(8) . ?
C1 C2 1.386(8) . ?
C1 C5 1.508(8) . ?
C1 H1 0.9500 . ?
C2 C3 1.397(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.371(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.522(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.556(9) . ?
C5 H5 1.0000 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.520(9) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.471(10) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.414(10) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.186(15) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.517(9) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.381(11) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.403(9) . ?
C19 C23 1.453(9) . ?
C19 H19 0.9500 . ?
C20 C21 1.363(9) . ?
C20 H20 0.9500 . ?
C21 C22 1.376(9) . ?
C21 H21 0.9500 . ?
C22 C23 1.540(10) . ?
C22 H22 0.9500 . ?
C23 C24 1.569(9) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.233(14) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.398(12) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.467(11) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.379(9) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.476(10) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.509(10) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O2 Zr1 O2 180.0 . 2_556 ?
O2 Zr1 O1 87.66(15) . . ?
O2 Zr1 O1 92.34(15) 2_556 . ?
O2 Zr1 O1 92.34(15) . 2_556 ?
O2 Zr1 O1 87.66(15) 2_556 2_556 ?
O1 Zr1 O1 180.0 . 2_556 ?
O2 Zr1 O3 88.40(15) . . ?
O2 Zr1 O3 91.60(15) 2_556 . ?
O1 Zr1 O3 87.58(14) . . ?
O1 Zr1 O3 92.42(14) 2_556 . ?
O2 Zr1 O3 91.60(15) . 2_556 ?
O2 Zr1 O3 88.40(15) 2_556 2_556 ?
O1 Zr1 O3 92.42(14) . 2_556 ?
O1 Zr1 O3 87.58(14) 2_556 2_556 ?
O3 Zr1 O3 180.0 . 2_556 ?
O12 Zr2 O12 180.0(3) . 2_665 ?
O12 Zr2 O10 92.22(17) . . ?
O12 Zr2 O10 87.78(17) 2_665 . ?
O12 Zr2 O10 87.78(17) . 2_665 ?
O12 Zr2 O10 92.22(17) 2_665 2_665 ?
O10 Zr2 O10 180.0(2) . 2_665 ?
O12 Zr2 O11 92.77(16) . 2_665 ?
O12 Zr2 O11 87.23(16) 2_665 2_665 ?
O10 Zr2 O11 88.26(16) . 2_665 ?
O10 Zr2 O11 91.74(16) 2_665 2_665 ?
O12 Zr2 O11 87.23(16) . . ?
O12 Zr2 O11 92.77(16) 2_665 . ?
O10 Zr2 O11 91.74(16) . . ?
O10 Zr2 O11 88.26(16) 2_665 . ?
O11 Zr2 O11 180.000(1) 2_665 . ?
C3 Co1 C2 40.9(2) . . ?
C3 Co1 C4 39.6(2) . . ?
C2 Co1 C4 66.0(2) . . ?
C3 Co1 C1 67.1(3) . . ?
C2 Co1 C1 39.7(2) . . ?
C4 Co1 C1 64.4(2) . . ?
C3 Co1 P3 94.33(19) . . ?
C2 Co1 P3 126.71(18) . . ?
C4 Co1 P3 99.12(18) . . ?
C1 Co1 P3 161.05(19) . . ?
C3 Co1 P2 140.00(19) . . ?
C2 Co1 P2 136.07(18) . . ?
C4 Co1 P2 100.51(18) . . ?
C1 Co1 P2 96.37(18) . . ?
P3 Co1 P2 95.88(7) . . ?
C3 Co1 P1 123.59(19) . . ?
C2 Co1 P1 93.96(19) . . ?
C4 Co1 P1 159.99(18) . . ?
C1 Co1 P1 101.03(18) . . ?
P3 Co1 P1 92.35(7) . . ?
P2 Co1 P1 94.52(7) . . ?
C20 Co2 C21 40.0(3) . . ?
C20 Co2 C19 40.4(3) . . ?
C21 Co2 C19 66.8(3) . . ?
C20 Co2 C22 66.4(3) . . ?
C21 Co2 C22 39.4(3) . . ?
C19 Co2 C22 65.4(3) . . ?
C20 Co2 P5 96.28(19) . 2_665 ?
C21 Co2 P5 125.9(2) . 2_665 ?
C19 Co2 P5 102.0(2) . 2_665 ?
C22 Co2 P5 162.7(2) . 2_665 ?
C20 Co2 P4 141.1(2) . . ?
C21 Co2 P4 137.9(2) . . ?
C19 Co2 P4 100.8(2) . . ?
C22 Co2 P4 98.4(2) . . ?
P5 Co2 P4 95.57(8) 2_665 . ?
C20 Co2 P6 122.0(2) . 2_665 ?
C21 Co2 P6 92.3(2) . 2_665 ?
C19 Co2 P6 159.1(2) . 2_665 ?
C22 Co2 P6 98.8(2) . 2_665 ?
P5 Co2 P6 90.15(8) 2_665 2_665 ?
P4 Co2 P6 94.81(8) . 2_665 ?
O1 P1 O5 104.2(2) . . ?
O1 P1 O4 106.6(2) . . ?
O5 P1 O4 99.0(2) . . ?
O1 P1 Co1 115.46(16) . . ?
O5 P1 Co1 120.58(17) . . ?
O4 P1 Co1 109.14(17) . . ?
O2 P2 O6 104.5(2) . . ?
O2 P2 O7 105.2(2) . . ?
O6 P2 O7 101.0(2) . . ?
O2 P2 Co1 115.62(16) . . ?
O6 P2 Co1 113.39(16) . . ?
O7 P2 Co1 115.49(16) . . ?
O3 P3 O8 105.7(2) . . ?
O3 P3 O9 105.0(2) . . ?
O8 P3 O9 98.0(2) . . ?
O3 P3 Co1 116.71(16) . . ?
O8 P3 Co1 114.42(16) . . ?
O9 P3 Co1 114.86(18) . . ?
O10 P4 O13 105.6(2) . . ?
O10 P4 O14 104.2(3) . . ?
O13 P4 O14 96.7(3) . . ?
O10 P4 Co2 113.86(18) . . ?
O13 P4 Co2 114.41(19) . . ?
O14 P4 Co2 119.9(2) . . ?
O11 P5 O16 104.9(2) . . ?
O11 P5 O15 105.6(2) . . ?
O16 P5 O15 98.6(2) . . ?
O11 P5 Co2 115.80(18) . 2_665 ?
O16 P5 Co2 118.09(19) . 2_665 ?
O15 P5 Co2 111.82(18) . 2_665 ?
O12 P6 O17 106.8(2) . . ?
O12 P6 O18 104.7(2) . . ?
O17 P6 O18 99.0(3) . . ?
O12 P6 Co2 114.88(19) . 2_665 ?
O17 P6 Co2 112.96(18) . 2_665 ?
O18 P6 Co2 116.92(19) . 2_665 ?
P1 O1 Zr1 133.1(2) . . ?
P2 O2 Zr1 132.9(2) . . ?
P3 O3 Zr1 131.7(2) . . ?
C7 O4 P1 119.6(4) . . ?
C9 O5 P1 123.2(4) . . ?
C11 O6 P2 121.4(4) . . ?
C13 O7 P2 127.7(6) . . ?
C15 O8 P3 119.9(4) . . ?
C17 O9 P3 121.1(4) . . ?
P4 O10 Zr2 131.4(3) . . ?
P5 O11 Zr2 129.8(2) . . ?
P6 O12 Zr2 128.2(2) . . ?
C25 O13 P4 119.6(5) . . ?
C27 O14 P4 122.0(5) . . ?
C29 O15 P5 119.9(5) . . ?
C31 O16 P5 127.2(5) . . ?
C33 O17 P6 118.5(4) . . ?
C35 O18 P6 123.6(5) . . ?
C2 C1 C5 109.5(6) . . ?
C2 C1 Co1 67.6(3) . . ?
C5 C1 Co1 92.7(4) . . ?
C2 C1 H1 125.3 . . ?
C5 C1 H1 125.3 . . ?
Co1 C1 H1 106.8 . . ?
C1 C2 C3 107.7(5) . . ?
C1 C2 Co1 72.7(3) . . ?
C3 C2 Co1 69.1(3) . . ?
C1 C2 H2 126.1 . . ?
C3 C2 H2 126.1 . . ?
Co1 C2 H2 123.6 . . ?
C4 C3 C2 106.0(6) . . ?
C4 C3 Co1 72.4(4) . . ?
C2 C3 Co1 70.0(3) . . ?
C4 C3 H3 127.0 . . ?
C2 C3 H3 127.0 . . ?
Co1 C3 H3 122.4 . . ?
C3 C4 C5 111.0(5) . . ?
C3 C4 Co1 68.0(4) . . ?
C5 C4 Co1 93.0(4) . . ?
C3 C4 H4 124.5 . . ?
C5 C4 H4 124.5 . . ?
Co1 C4 H4 106.5 . . ?
C1 C5 C4 92.9(5) . . ?
C1 C5 C6 115.3(5) . . ?
C4 C5 C6 115.0(6) . . ?
C1 C5 H5 110.8 . . ?
C4 C5 H5 110.8 . . ?
C6 C5 H5 110.8 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O4 C7 C8 108.3(6) . . ?
O4 C7 H7A 110.0 . . ?
C8 C7 H7A 110.0 . . ?
O4 C7 H7B 110.0 . . ?
C8 C7 H7B 110.0 . . ?
H7A C7 H7B 108.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O5 C9 C10 108.2(6) . . ?
O5 C9 H9A 110.1 . . ?
C10 C9 H9A 110.1 . . ?
O5 C9 H9B 110.1 . . ?
C10 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O6 C11 C12 112.4(6) . . ?
O6 C11 H11A 109.1 . . ?
C12 C11 H11A 109.1 . . ?
O6 C11 H11B 109.1 . . ?
C12 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 O7 144.2(13) . . ?
C14 C13 H13A 100.9 . . ?
O7 C13 H13A 100.9 . . ?
C14 C13 H13B 100.9 . . ?
O7 C13 H13B 100.9 . . ?
H13A C13 H13B 104.4 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O8 C15 C16 109.4(5) . . ?
O8 C15 H15A 109.8 . . ?
C16 C15 H15A 109.8 . . ?
O8 C15 H15B 109.8 . . ?
C16 C15 H15B 109.8 . . ?
H15A C15 H15B 108.2 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 O9 111.3(7) . . ?
C18 C17 H17A 109.4 . . ?
O9 C17 H17A 109.4 . . ?
C18 C17 H17B 109.4 . . ?
O9 C17 H17B 109.4 . . ?
H17A C17 H17B 108.0 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C23 108.4(6) . . ?
C20 C19 Co2 66.5(4) . . ?
C23 C19 Co2 91.8(5) . . ?
C20 C19 H19 125.8 . . ?
C23 C19 H19 125.8 . . ?
Co2 C19 H19 108.3 . . ?
C21 C20 C19 108.2(6) . . ?
C21 C20 Co2 70.6(4) . . ?
C19 C20 Co2 73.1(4) . . ?
C21 C20 H20 125.9 . . ?
C19 C20 H20 125.9 . . ?
Co2 C20 H20 122.1 . . ?
C20 C21 C22 108.6(7) . . ?
C20 C21 Co2 69.4(4) . . ?
C22 C21 Co2 73.3(4) . . ?
C20 C21 H21 125.7 . . ?
C22 C21 H21 125.7 . . ?
Co2 C21 H21 123.2 . . ?
C21 C22 C23 106.7(6) . . ?
C21 C22 Co2 67.3(4) . . ?
C23 C22 Co2 89.2(5) . . ?
C21 C22 H22 126.6 . . ?
C23 C22 H22 126.6 . . ?
Co2 C22 H22 109.6 . . ?
C19 C23 C22 96.8(5) . . ?
C19 C23 C24 116.2(6) . . ?
C22 C23 C24 109.7(6) . . ?
C19 C23 H23 111.1 . . ?
C22 C23 H23 111.1 . . ?
C24 C23 H23 111.1 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 O13 120.2(12) . . ?
C26 C25 H25A 107.3 . . ?
O13 C25 H25A 107.3 . . ?
C26 C25 H25B 107.3 . . ?
O13 C25 H25B 107.3 . . ?
H25A C25 H25B 106.9 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O14 C27 C28 113.0(8) . . ?
O14 C27 H27A 109.0 . . ?
C28 C27 H27A 109.0 . . ?
O14 C27 H27B 109.0 . . ?
C28 C27 H27B 109.0 . . ?
H27A C27 H27B 107.8 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O15 C29 C30 112.7(7) . . ?
O15 C29 H29A 109.0 . . ?
C30 C29 H29A 109.0 . . ?
O15 C29 H29B 109.0 . . ?
C30 C29 H29B 109.0 . . ?
H29A C29 H29B 107.8 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O16 C31 C32 116.8(8) . . ?
O16 C31 H31A 108.1 . . ?
C32 C31 H31A 108.1 . . ?
O16 C31 H31B 108.1 . . ?
C32 C31 H31B 108.1 . . ?
H31A C31 H31B 107.3 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 O17 110.6(6) . . ?
C34 C33 H33A 109.5 . . ?
O17 C33 H33A 109.5 . . ?
C34 C33 H33B 109.5 . . ?
O17 C33 H33B 109.5 . . ?
H33A C33 H33B 108.1 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O18 C35 C36 108.5(6) . . ?
O18 C35 H35A 110.0 . . ?
C36 C35 H35A 110.0 . . ?
O18 C35 H35B 110.0 . . ?
C36 C35 H35B 110.0 . . ?
H35A C35 H35B 108.4 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
 
_diffrn_measured_fraction_theta_max    0.754
_diffrn_reflns_theta_full              25.13
_diffrn_measured_fraction_theta_full   0.754
_refine_diff_density_max    1.235
_refine_diff_density_min   -0.453
_refine_diff_density_rms    0.112
