data_s93
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr. Craig Matthews
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C44 H46 Cl4 Co2 N16 O21'
_chemical_formula_weight          1394.63
 
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'
 'N'  'N'   0.0061   0.0033
 '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'
 'Cl'  'Cl'   0.1484   0.1585
 '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'
 
_symmetry_cell_setting            Orthorhombic
_symmetry_space_group_name_H-M    Pna2(1)
_symmetry_space_group_name_hall   'P 2c -2n'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, z+1/2'
 'x+1/2, -y+1/2, z'
 '-x+1/2, y+1/2, z+1/2'
 
_cell_length_a                    25.808(5)
_cell_length_b                    11.9889(8)
_cell_length_c                    17.384(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      5378.8(15)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     12522
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Block
_exptl_crystal_colour             Red
_exptl_crystal_size_max           0.36
_exptl_crystal_size_mid           0.24
_exptl_crystal_size_min           0.16
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.722
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              2848
_exptl_absorpt_coefficient_mu     0.912
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.7349
_exptl_absorpt_correction_T_max   0.8678
_exptl_absorpt_process_details    'SORTAV Blessing (1997)'
 
_exptl_special_details
;
 PLEASE NOTE cell_measurement_ fields are not relevant to area detector data,
 the entire data set is used to refine the cell, which is indexed from all
 observed reflections in a 10 degree phi range.
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Nonius KappaCCD Area Detector'
_diffrn_measurement_method        'φ and ω scans to fill Ewald Sphere'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             72712
_diffrn_reflns_av_R_equivalents   0.0606
_diffrn_reflns_av_sigmaI/netI     0.0525
_diffrn_reflns_limit_h_min        -32
_diffrn_reflns_limit_h_max        33
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -22
_diffrn_reflns_limit_l_max        22
_diffrn_reflns_theta_min          3.00
_diffrn_reflns_theta_max          27.48
_reflns_number_total              12146
_reflns_number_gt                 9321
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection
' DENZO (Otwinowski and Minor, 1997)'
_computing_cell_refinement        
' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_data_reduction         
' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997b)' 
_computing_molecular_graphics     'PLATON (Spek, 1990)'
_computing_publication_material   ? 
 
_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 > 2sigma(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)+(0.0724P)²+11.8958P] 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_abs_structure_details
 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    0.48(2)
_refine_ls_number_reflns          12146
_refine_ls_number_parameters      786
_refine_ls_number_restraints      71
_refine_ls_R_factor_all           0.0827
_refine_ls_R_factor_gt            0.0568
_refine_ls_wR_factor_ref          0.1512
_refine_ls_wR_factor_gt           0.1381
_refine_ls_goodness_of_fit_ref    1.022
_refine_ls_restrained_S_all       1.024
_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
C1 C 0.3525(3) 0.3911(6) 0.1450(4) 0.0312(15) Uani 1 1 d . . .
H1 H 0.3429 0.3508 0.1899 0.037 Uiso 1 1 calc R . .
C2 C 0.3903(2) 0.4709(5) 0.1516(4) 0.0291(15) Uani 1 1 d . . .
H2 H 0.4061 0.4853 0.1999 0.035 Uiso 1 1 calc R . .
C3 C 0.4049(3) 0.5287(6) 0.0882(4) 0.0323(16) Uani 1 1 d . . .
H3 H 0.4312 0.5840 0.0912 0.039 Uiso 1 1 calc R . .
C4 C 0.3803(3) 0.5055(5) 0.0187(4) 0.0294(15) Uani 1 1 d . . .
H4 H 0.3896 0.5454 -0.0265 0.035 Uiso 1 1 calc R . .
C5 C 0.3433(2) 0.4260(5) 0.0157(4) 0.0213(13) Uani 1 1 d . . .
C6 C 0.3144(2) 0.3951(5) -0.0542(3) 0.0196(12) Uani 1 1 d . . .
C7 C 0.3253(2) 0.4393(5) -0.1265(4) 0.0252(13) Uani 1 1 d . . .
H7 H 0.3528 0.4909 -0.1338 0.030 Uiso 1 1 calc R . .
C8 C 0.2946(3) 0.4052(5) -0.1870(4) 0.0276(14) Uani 1 1 d . . .
H8 H 0.3009 0.4340 -0.2371 0.033 Uiso 1 1 calc R . .
C9 C 0.2549(2) 0.3300(5) -0.1759(4) 0.0244(13) Uani 1 1 d . . .
H9 H 0.2343 0.3049 -0.2177 0.029 Uiso 1 1 calc R . .
C10 C 0.2462(2) 0.2921(5) -0.1012(3) 0.0202(12) Uani 1 1 d . . .
C11 C 0.2044(2) 0.2174(5) -0.0776(3) 0.0191(12) Uani 1 1 d . . .
C12 C 0.1674(2) 0.0413(4) 0.0590(4) 0.0206(11) Uani 1 1 d . . .
C13 C 0.1215(2) 0.0123(5) 0.1043(4) 0.0194(12) Uani 1 1 d . . .
C14 C 0.1074(2) -0.0922(5) 0.1283(4) 0.0259(14) Uani 1 1 d . . .
H14 H 0.1277 -0.1559 0.1161 0.031 Uiso 1 1 calc R . .
C15 C 0.0620(2) -0.1011(6) 0.1713(4) 0.0265(14) Uani 1 1 d . . .
H15 H 0.0498 -0.1725 0.1865 0.032 Uiso 1 1 calc R . .
C16 C 0.0354(2) -0.0088(5) 0.1914(4) 0.0250(13) Uani 1 1 d . . .
H16 H 0.0059 -0.0153 0.2239 0.030 Uiso 1 1 calc R . .
C17 C 0.0504(2) 0.0944(5) 0.1654(3) 0.0210(13) Uani 1 1 d . . .
C18 C 0.0250(2) 0.2028(6) 0.1796(4) 0.0259(14) Uani 1 1 d . . .
C19 C -0.0164(2) 0.2143(6) 0.2270(4) 0.0281(14) Uani 1 1 d . . .
H19 H -0.0322 0.1512 0.2503 0.034 Uiso 1 1 calc R . .
C20 C -0.0348(2) 0.3199(6) 0.2402(4) 0.0284(14) Uani 1 1 d . . .
H20 H -0.0635 0.3312 0.2735 0.034 Uiso 1 1 calc R . .
C21 C -0.0119(2) 0.4078(6) 0.2055(4) 0.0290(15) Uani 1 1 d . . .
H21 H -0.0239 0.4815 0.2150 0.035 Uiso 1 1 calc R . .
C22 C 0.0285(3) 0.3896(6) 0.1567(4) 0.0287(15) Uani 1 1 d . . .
H22 H 0.0445 0.4516 0.1324 0.034 Uiso 1 1 calc R . .
C31 C 0.3478(2) 0.0961(5) -0.0306(4) 0.0273(14) Uani 1 1 d . . .
H31 H 0.3338 0.1299 -0.0755 0.033 Uiso 1 1 calc R . .
C32 C 0.3890(2) 0.0229(5) -0.0381(4) 0.0267(14) Uani 1 1 d . . .
H32 H 0.4031 0.0060 -0.0872 0.032 Uiso 1 1 calc R . .
C33 C 0.4086(3) -0.0235(5) 0.0259(4) 0.0313(16) Uani 1 1 d . . .
H33 H 0.4367 -0.0745 0.0225 0.038 Uiso 1 1 calc R . .
C34 C 0.3879(3) 0.0030(5) 0.0960(4) 0.0312(15) Uani 1 1 d . . .
H34 H 0.4022 -0.0270 0.1419 0.037 Uiso 1 1 calc R . .
C35 C 0.3458(2) 0.0740(5) 0.0990(4) 0.0199(12) Uani 1 1 d . . .
C36 C 0.3186(2) 0.0988(5) 0.1713(4) 0.0210(13) Uani 1 1 d . . .
C37 C 0.3298(3) 0.0584(5) 0.2437(4) 0.0281(14) Uani 1 1 d . . .
H37 H 0.3571 0.0065 0.2510 0.034 Uiso 1 1 calc R . .
C38 C 0.3014(2) 0.0934(5) 0.3040(4) 0.0285(14) Uani 1 1 d . . .
H38 H 0.3099 0.0687 0.3544 0.034 Uiso 1 1 calc R . .
C39 C 0.2598(2) 0.1650(5) 0.2936(4) 0.0254(14) Uani 1 1 d . . .
H39 H 0.2388 0.1879 0.3356 0.031 Uiso 1 1 calc R . .
C40 C 0.2502(2) 0.2011(4) 0.2211(4) 0.0194(12) Uani 1 1 d . . .
C41 C 0.2063(2) 0.2722(5) 0.1957(3) 0.0166(12) Uani 1 1 d . . .
C42 C 0.16789(19) 0.4476(4) 0.0611(4) 0.0166(10) Uani 1 1 d . . .
C43 C 0.1218(2) 0.4744(5) 0.0121(4) 0.0193(12) Uani 1 1 d . . .
C44 C 0.1088(3) 0.5782(5) -0.0132(4) 0.0255(13) Uani 1 1 d . . .
H44 H 0.1294 0.6414 -0.0008 0.031 Uiso 1 1 calc R . .
C45 C 0.0647(3) 0.5881(6) -0.0572(4) 0.0330(17) Uani 1 1 d . . .
H45 H 0.0543 0.6592 -0.0756 0.040 Uiso 1 1 calc R . .
C46 C 0.0357(2) 0.4945(5) -0.0748(4) 0.0304(15) Uani 1 1 d . . .
H46 H 0.0057 0.4997 -0.1063 0.037 Uiso 1 1 calc R . .
C47 C 0.0515(2) 0.3948(5) -0.0455(4) 0.0233(13) Uani 1 1 d . . .
C48 C 0.0254(2) 0.2884(5) -0.0601(3) 0.0210(12) Uani 1 1 d . . .
C49 C -0.0165(3) 0.2742(6) -0.1084(4) 0.0278(14) Uani 1 1 d . . .
H49 H -0.0318 0.3365 -0.1334 0.033 Uiso 1 1 calc R . .
C50 C -0.0358(3) 0.1685(6) -0.1198(4) 0.0346(16) Uani 1 1 d . . .
H50 H -0.0652 0.1584 -0.1520 0.042 Uiso 1 1 calc R . .
C51 C -0.0137(3) 0.0783(6) -0.0859(4) 0.0337(16) Uani 1 1 d . . .
H51 H -0.0262 0.0050 -0.0950 0.040 Uiso 1 1 calc R . .
C52 C 0.0278(2) 0.0979(5) -0.0377(4) 0.0262(14) Uani 1 1 d . . .
H52 H 0.0434 0.0358 -0.0128 0.031 Uiso 1 1 calc R . .
N1 N 0.32831(18) 0.3669(4) 0.0794(3) 0.0248(12) Uani 1 1 d . . .
N2 N 0.27639(18) 0.3249(4) -0.0445(3) 0.0195(10) Uani 1 1 d . . .
N3 N 0.16393(19) 0.2053(4) -0.1235(3) 0.0248(11) Uani 1 1 d . . .
H3A H 0.1371 0.1656 -0.1083 0.030 Uiso 1 1 calc R . .
H3B H 0.1638 0.2369 -0.1692 0.030 Uiso 1 1 calc R . .
N4 N 0.20982(18) 0.1759(4) -0.0095(3) 0.0179(10) Uani 1 1 d . . .
N5 N 0.16367(18) 0.1360(4) 0.0217(3) 0.0205(10) Uani 1 1 d . . .
N6 N 0.20861(17) -0.0234(3) 0.0591(3) 0.0224(10) Uani 1 1 d . . .
H6A H 0.2363 -0.0040 0.0327 0.027 Uiso 1 1 calc R . .
H6B H 0.2085 -0.0860 0.0855 0.027 Uiso 1 1 calc R . .
N7 N 0.09363(19) 0.1022(4) 0.1222(3) 0.0213(11) Uani 1 1 d . . .
N8 N 0.0462(2) 0.2883(4) 0.1422(3) 0.0226(11) Uani 1 1 d . . .
N31 N 0.32753(19) 0.1202(4) 0.0366(3) 0.0222(11) Uani 1 1 d . . .
N32 N 0.27920(17) 0.1697(4) 0.1604(3) 0.0176(10) Uani 1 1 d . . .
N33 N 0.1667(2) 0.2893(4) 0.2422(3) 0.0280(11) Uani 1 1 d . . .
H33A H 0.1403 0.3302 0.2268 0.034 Uiso 1 1 calc R . .
H33B H 0.1666 0.2599 0.2885 0.034 Uiso 1 1 calc R . .
N34 N 0.21035(17) 0.3112(4) 0.1271(3) 0.0179(10) Uani 1 1 d . . .
N35 N 0.16364(17) 0.3532(4) 0.0971(3) 0.0191(10) Uani 1 1 d . . .
N36 N 0.20860(17) 0.5131(4) 0.0592(4) 0.0243(10) Uani 1 1 d . . .
H36A H 0.2369 0.4943 0.0842 0.029 Uiso 1 1 calc R . .
H36B H 0.2076 0.5758 0.0329 0.029 Uiso 1 1 calc R . .
N37 N 0.09331(17) 0.3860(4) -0.0032(3) 0.0165(9) Uani 1 1 d . . .
N38 N 0.04717(19) 0.1992(4) -0.0240(3) 0.0206(10) Uani 1 1 d . . .
Co1 Co 0.269734(19) 0.24571(6) 0.05817(7) 0.01721(13) Uani 1 1 d . . .
Co2 Co 0.10409(2) 0.24426(6) 0.05939(7) 0.01724(13) Uani 1 1 d . . .
O1 O 0.43429(17) 0.6713(4) 0.2656(3) 0.0331(12) Uani 1 1 d D . .
O2 O 0.42450(18) 0.8643(4) 0.2712(3) 0.0321(11) Uani 1 1 d D . .
O3 O 0.4455(2) 0.7793(5) 0.1553(3) 0.0461(14) Uani 1 1 d D . .
O4 O 0.3638(2) 0.7589(4) 0.2076(4) 0.0422(15) Uani 1 1 d D . .
Cl1 Cl 0.41851(7) 0.76780(13) 0.22501(10) 0.0276(4) Uani 1 1 d D . .
O11 O 0.07741(19) 0.1350(4) 0.3423(3) 0.0336(11) Uani 1 1 d D . .
O12 O 0.0652(2) 0.3283(4) 0.3447(3) 0.0399(14) Uani 1 1 d D . .
O13 O 0.1370(2) 0.2453(4) 0.4036(4) 0.0407(15) Uani 1 1 d D . .
O14 O 0.0558(2) 0.2238(5) 0.4574(3) 0.0520(16) Uani 1 1 d D . .
Cl11 Cl 0.08187(7) 0.23295(13) 0.38711(10) 0.0293(4) Uani 1 1 d D . .
O21 O 0.30977(17) 0.3980(5) 0.3886(3) 0.0577(14) Uani 1 1 d D . .
O22 O 0.3867(2) 0.3524(5) 0.4516(3) 0.0635(17) Uani 1 1 d D . .
O23 O 0.3867(2) 0.4820(4) 0.3542(4) 0.0682(18) Uani 1 1 d D . .
O24 O 0.3744(2) 0.2975(5) 0.3251(3) 0.0517(14) Uani 1 1 d D . .
Cl21 Cl 0.36397(7) 0.38207(12) 0.37889(9) 0.0361(4) Uani 1 1 d D . .
O31 O 0.1317(2) 0.7040(4) 0.2836(4) 0.0588(17) Uani 1 1 d D . .
O32 O 0.1224(3) 0.6395(5) 0.1614(3) 0.077(2) Uani 1 1 d D . .
O33 O 0.1401(3) 0.5163(4) 0.2573(4) 0.082(2) Uani 1 1 d D . .
O34 O 0.05997(19) 0.6006(6) 0.2517(4) 0.091(2) Uani 1 1 d D . .
Cl31 Cl 0.11518(8) 0.61458(13) 0.23800(10) 0.0459(4) Uani 1 1 d D . .
O51 O 0.2696(2) 0.2041(4) 0.4720(3) 0.0423(12) Uani 1 1 d . . .
O52 O 0.2427(2) 0.5398(5) 0.3106(4) 0.0741(17) Uani 1 1 d . . .
O53 O 0.28045(19) 0.6016(4) 0.1724(3) 0.0545(13) Uani 1 1 d . . .
O54 O 0.2171(2) 0.7813(5) 0.1513(3) 0.0538(15) Uani 1 1 d . . .
O55 O 0.3167(2) 0.7918(5) 0.0466(3) 0.0696(17) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds 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
C1 N1 1.333(8) . ?
C1 C2 1.371(9) . ?
C1 H1 0.9500 . ?
C2 C3 1.354(9) . ?
C2 H2 0.9500 . ?
C3 C4 1.393(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.351(9) . ?
C4 H4 0.9500 . ?
C5 N1 1.369(8) . ?
C5 C6 1.473(9) . ?
C6 N2 1.304(7) . ?
C6 C7 1.393(8) . ?
C7 C8 1.379(9) . ?
C7 H7 0.9500 . ?
C8 C9 1.379(9) . ?
C8 H8 0.9500 . ?
C9 C10 1.394(8) . ?
C9 H9 0.9500 . ?
C10 N2 1.317(8) . ?
C10 C11 1.461(9) . ?
C11 N4 1.292(7) . ?
C11 N3 1.321(8) . ?
C12 N5 1.311(7) . ?
C12 N6 1.317(7) . ?
C12 C13 1.463(8) . ?
C13 N7 1.332(7) . ?
C13 C14 1.370(8) . ?
C14 C15 1.394(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.349(9) . ?
C15 H15 0.9500 . ?
C16 C17 1.374(8) . ?
C16 H16 0.9500 . ?
C17 N7 1.348(8) . ?
C17 C18 1.476(9) . ?
C18 N8 1.330(9) . ?
C18 C19 1.358(9) . ?
C19 C20 1.371(9) . ?
C19 H19 0.9500 . ?
C20 C21 1.349(9) . ?
C20 H20 0.9500 . ?
C21 C22 1.362(9) . ?
C21 H21 0.9500 . ?
C22 N8 1.321(8) . ?
C22 H22 0.9500 . ?
C31 N31 1.312(8) . ?
C31 C32 1.386(9) . ?
C31 H31 0.9500 . ?
C32 C33 1.342(9) . ?
C32 H32 0.9500 . ?
C33 C34 1.368(10) . ?
C33 H33 0.9500 . ?
C34 C35 1.381(9) . ?
C34 H34 0.9500 . ?
C35 N31 1.306(8) . ?
C35 C36 1.470(9) . ?
C36 N32 1.339(7) . ?
C36 C37 1.379(9) . ?
C37 C38 1.346(10) . ?
C37 H37 0.9500 . ?
C38 C39 1.387(9) . ?
C38 H38 0.9500 . ?
C39 C40 1.354(9) . ?
C39 H39 0.9500 . ?
C40 N32 1.348(8) . ?
C40 C41 1.486(8) . ?
C41 N34 1.285(7) . ?
C41 N33 1.319(8) . ?
C42 N35 1.298(7) . ?
C42 N36 1.312(6) . ?
C42 C43 1.498(8) . ?
C43 N37 1.316(7) . ?
C43 C44 1.361(8) . ?
C44 C45 1.376(9) . ?
C44 H44 0.9500 . ?
C45 C46 1.383(10) . ?
C45 H45 0.9500 . ?
C46 C47 1.362(9) . ?
C46 H46 0.9500 . ?
C47 N37 1.312(8) . ?
C47 C48 1.464(9) . ?
C48 N38 1.361(8) . ?
C48 C49 1.380(9) . ?
C49 C50 1.376(10) . ?
C49 H49 0.9500 . ?
C50 C51 1.357(10) . ?
C50 H50 0.9500 . ?
C51 C52 1.380(9) . ?
C51 H51 0.9500 . ?
C52 N38 1.335(8) . ?
C52 H52 0.9500 . ?
N1 Co1 2.129(5) . ?
N2 Co1 2.029(5) . ?
N3 H3A 0.8800 . ?
N3 H3B 0.8800 . ?
N4 N5 1.393(7) . ?
N4 Co1 2.116(5) . ?
N5 Co2 2.117(5) . ?
N6 H6A 0.8800 . ?
N6 H6B 0.8800 . ?
N7 Co2 2.041(5) . ?
N8 Co2 2.141(5) . ?
N31 Co1 2.152(5) . ?
N32 Co1 2.012(5) . ?
N33 H33A 0.8800 . ?
N33 H33B 0.8800 . ?
N34 N35 1.407(6) . ?
N34 Co1 2.097(5) . ?
N35 Co2 2.120(5) . ?
N36 H36A 0.8800 . ?
N36 H36B 0.8800 . ?
N37 Co2 2.037(5) . ?
N38 Co2 2.133(5) . ?
O1 Cl1 1.415(4) . ?
O2 Cl1 1.416(4) . ?
O3 Cl1 1.404(5) . ?
O4 Cl1 1.448(5) . ?
O11 Cl11 1.414(5) . ?
O12 Cl11 1.426(5) . ?
O13 Cl11 1.460(5) . ?
O14 Cl11 1.400(5) . ?
O21 Cl21 1.422(5) . ?
O22 Cl21 1.438(5) . ?
O23 Cl21 1.401(5) . ?
O24 Cl21 1.406(5) . ?
O31 Cl31 1.399(5) . ?
O32 Cl31 1.377(6) . ?
O33 Cl31 1.383(5) . ?
O34 Cl31 1.454(5) . ?
 
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
N1 C1 C2 123.8(7) . . ?
N1 C1 H1 118.1 . . ?
C2 C1 H1 118.1 . . ?
C3 C2 C1 119.1(7) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C2 C3 C4 118.5(6) . . ?
C2 C3 H3 120.7 . . ?
C4 C3 H3 120.7 . . ?
C5 C4 C3 119.7(6) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 N1 122.3(6) . . ?
C4 C5 C6 124.5(6) . . ?
N1 C5 C6 113.2(5) . . ?
N2 C6 C7 120.9(6) . . ?
N2 C6 C5 115.9(5) . . ?
C7 C6 C5 123.2(5) . . ?
C8 C7 C6 117.4(5) . . ?
C8 C7 H7 121.3 . . ?
C6 C7 H7 121.3 . . ?
C9 C8 C7 120.9(6) . . ?
C9 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
C8 C9 C10 117.7(6) . . ?
C8 C9 H9 121.2 . . ?
C10 C9 H9 121.2 . . ?
N2 C10 C9 120.2(6) . . ?
N2 C10 C11 114.2(5) . . ?
C9 C10 C11 125.5(6) . . ?
N4 C11 N3 126.6(6) . . ?
N4 C11 C10 114.4(5) . . ?
N3 C11 C10 118.8(5) . . ?
N5 C12 N6 124.7(6) . . ?
N5 C12 C13 114.4(5) . . ?
N6 C12 C13 120.9(5) . . ?
N7 C13 C14 121.7(6) . . ?
N7 C13 C12 111.8(5) . . ?
C14 C13 C12 126.6(5) . . ?
C13 C14 C15 117.1(6) . . ?
C13 C14 H14 121.4 . . ?
C15 C14 H14 121.4 . . ?
C16 C15 C14 120.3(6) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 C17 120.7(6) . . ?
C15 C16 H16 119.7 . . ?
C17 C16 H16 119.7 . . ?
N7 C17 C16 118.6(6) . . ?
N7 C17 C18 113.6(5) . . ?
C16 C17 C18 127.8(5) . . ?
N8 C18 C19 122.8(7) . . ?
N8 C18 C17 114.5(6) . . ?
C19 C18 C17 122.7(6) . . ?
C18 C19 C20 117.9(7) . . ?
C18 C19 H19 121.1 . . ?
C20 C19 H19 121.1 . . ?
C21 C20 C19 119.7(6) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
C20 C21 C22 119.2(6) . . ?
C20 C21 H21 120.4 . . ?
C22 C21 H21 120.4 . . ?
N8 C22 C21 122.1(6) . . ?
N8 C22 H22 119.0 . . ?
C21 C22 H22 119.0 . . ?
N31 C31 C32 121.9(6) . . ?
N31 C31 H31 119.0 . . ?
C32 C31 H31 119.0 . . ?
C33 C32 C31 118.3(6) . . ?
C33 C32 H32 120.9 . . ?
C31 C32 H32 120.9 . . ?
C32 C33 C34 119.7(6) . . ?
C32 C33 H33 120.2 . . ?
C34 C33 H33 120.2 . . ?
C33 C34 C35 119.0(6) . . ?
C33 C34 H34 120.5 . . ?
C35 C34 H34 120.5 . . ?
N31 C35 C34 120.9(6) . . ?
N31 C35 C36 116.9(5) . . ?
C34 C35 C36 122.2(6) . . ?
N32 C36 C37 120.8(6) . . ?
N32 C36 C35 111.7(5) . . ?
C37 C36 C35 127.5(5) . . ?
C38 C37 C36 119.1(6) . . ?
C38 C37 H37 120.4 . . ?
C36 C37 H37 120.4 . . ?
C37 C38 C39 120.9(6) . . ?
C37 C38 H38 119.6 . . ?
C39 C38 H38 119.6 . . ?
C40 C39 C38 117.4(6) . . ?
C40 C39 H39 121.3 . . ?
C38 C39 H39 121.3 . . ?
N32 C40 C39 122.6(5) . . ?
N32 C40 C41 110.5(5) . . ?
C39 C40 C41 126.8(6) . . ?
N34 C41 N33 125.1(5) . . ?
N34 C41 C40 115.0(5) . . ?
N33 C41 C40 119.8(5) . . ?
N35 C42 N36 127.0(5) . . ?
N35 C42 C43 113.2(4) . . ?
N36 C42 C43 119.6(5) . . ?
N37 C43 C44 122.2(6) . . ?
N37 C43 C42 112.7(5) . . ?
C44 C43 C42 125.1(5) . . ?
C43 C44 C45 117.5(6) . . ?
C43 C44 H44 121.2 . . ?
C45 C44 H44 121.2 . . ?
C44 C45 C46 120.1(6) . . ?
C44 C45 H45 120.0 . . ?
C46 C45 H45 120.0 . . ?
C47 C46 C45 117.9(6) . . ?
C47 C46 H46 121.1 . . ?
C45 C46 H46 121.1 . . ?
N37 C47 C46 121.7(6) . . ?
N37 C47 C48 113.9(5) . . ?
C46 C47 C48 124.3(6) . . ?
N38 C48 C49 120.5(6) . . ?
N38 C48 C47 114.5(6) . . ?
C49 C48 C47 124.9(6) . . ?
C50 C49 C48 119.0(7) . . ?
C50 C49 H49 120.5 . . ?
C48 C49 H49 120.5 . . ?
C51 C50 C49 121.2(7) . . ?
C51 C50 H50 119.4 . . ?
C49 C50 H50 119.4 . . ?
C50 C51 C52 117.1(6) . . ?
C50 C51 H51 121.5 . . ?
C52 C51 H51 121.5 . . ?
N38 C52 C51 123.6(6) . . ?
N38 C52 H52 118.2 . . ?
C51 C52 H52 118.2 . . ?
C1 N1 C5 116.5(5) . . ?
C1 N1 Co1 129.0(4) . . ?
C5 N1 Co1 114.5(4) . . ?
C6 N2 C10 122.8(5) . . ?
C6 N2 Co1 118.6(4) . . ?
C10 N2 Co1 118.0(4) . . ?
C11 N3 H3A 120.0 . . ?
C11 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
C11 N4 N5 113.3(5) . . ?
C11 N4 Co1 115.9(4) . . ?
N5 N4 Co1 123.0(4) . . ?
C12 N5 N4 115.3(5) . . ?
C12 N5 Co2 115.5(4) . . ?
N4 N5 Co2 122.0(3) . . ?
C12 N6 H6A 120.0 . . ?
C12 N6 H6B 120.0 . . ?
H6A N6 H6B 120.0 . . ?
C13 N7 C17 121.5(5) . . ?
C13 N7 Co2 118.6(4) . . ?
C17 N7 Co2 117.7(4) . . ?
C22 N8 C18 118.2(6) . . ?
C22 N8 Co2 126.6(5) . . ?
C18 N8 Co2 115.1(4) . . ?
C35 N31 C31 120.2(5) . . ?
C35 N31 Co1 113.7(4) . . ?
C31 N31 Co1 125.8(4) . . ?
C36 N32 C40 119.1(5) . . ?
C36 N32 Co1 120.4(4) . . ?
C40 N32 Co1 119.9(4) . . ?
C41 N33 H33A 120.0 . . ?
C41 N33 H33B 120.0 . . ?
H33A N33 H33B 120.0 . . ?
C41 N34 N35 113.9(5) . . ?
C41 N34 Co1 117.0(4) . . ?
N35 N34 Co1 123.3(3) . . ?
C42 N35 N34 114.8(4) . . ?
C42 N35 Co2 116.7(4) . . ?
N34 N35 Co2 121.0(3) . . ?
C42 N36 H36A 120.0 . . ?
C42 N36 H36B 120.0 . . ?
H36A N36 H36B 120.0 . . ?
C47 N37 C43 120.6(5) . . ?
C47 N37 Co2 118.6(4) . . ?
C43 N37 Co2 119.2(4) . . ?
C52 N38 C48 118.5(6) . . ?
C52 N38 Co2 127.6(4) . . ?
C48 N38 Co2 113.5(4) . . ?
N32 Co1 N2 168.14(14) . . ?
N32 Co1 N34 75.74(19) . . ?
N2 Co1 N34 112.90(18) . . ?
N32 Co1 N4 113.64(18) . . ?
N2 Co1 N4 75.97(19) . . ?
N34 Co1 N4 86.07(13) . . ?
N32 Co1 N1 94.01(19) . . ?
N2 Co1 N1 76.87(19) . . ?
N34 Co1 N1 99.47(19) . . ?
N4 Co1 N1 152.27(19) . . ?
N32 Co1 N31 75.71(18) . . ?
N2 Co1 N31 96.62(18) . . ?
N34 Co1 N31 150.19(19) . . ?
N4 Co1 N31 97.64(18) . . ?
N1 Co1 N31 90.89(15) . . ?
N37 Co2 N7 164.55(14) . . ?
N37 Co2 N5 116.46(19) . . ?
N7 Co2 N5 75.51(19) . . ?
N37 Co2 N35 75.52(18) . . ?
N7 Co2 N35 116.40(19) . . ?
N5 Co2 N35 86.97(13) . . ?
N37 Co2 N38 75.78(19) . . ?
N7 Co2 N38 93.5(2) . . ?
N5 Co2 N38 97.72(19) . . ?
N35 Co2 N38 149.87(19) . . ?
N37 Co2 N8 93.31(19) . . ?
N7 Co2 N8 75.8(2) . . ?
N5 Co2 N8 150.1(2) . . ?
N35 Co2 N8 98.43(19) . . ?
N38 Co2 N8 92.19(14) . . ?
O3 Cl1 O1 111.6(3) . . ?
O3 Cl1 O2 110.8(4) . . ?
O1 Cl1 O2 110.7(3) . . ?
O3 Cl1 O4 108.1(4) . . ?
O1 Cl1 O4 108.9(3) . . ?
O2 Cl1 O4 106.6(3) . . ?
O14 Cl11 O11 112.1(4) . . ?
O14 Cl11 O12 111.6(3) . . ?
O11 Cl11 O12 110.9(3) . . ?
O14 Cl11 O13 107.8(4) . . ?
O11 Cl11 O13 105.8(3) . . ?
O12 Cl11 O13 108.3(3) . . ?
O23 Cl21 O24 109.5(4) . . ?
O23 Cl21 O21 109.4(4) . . ?
O24 Cl21 O21 111.4(3) . . ?
O23 Cl21 O22 108.0(4) . . ?
O24 Cl21 O22 109.1(4) . . ?
O21 Cl21 O22 109.3(4) . . ?
O32 Cl31 O33 110.9(4) . . ?
O32 Cl31 O31 109.9(4) . . ?
O33 Cl31 O31 111.9(4) . . ?
O32 Cl31 O34 108.4(5) . . ?
O33 Cl31 O34 108.5(5) . . ?
O31 Cl31 O34 107.1(4) . . ?
 
_diffrn_measured_fraction_theta_max    0.998
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.998
_refine_diff_density_max    1.414
_refine_diff_density_min   -1.270
_refine_diff_density_rms    0.098
