data_s92
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr. M. B. Smith
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C66 H58 N2 O6 P4 Pd, 2(Cl)'
_chemical_formula_sum
 'C66 H58 Cl2 N2 O6 P4 Pd'
_chemical_formula_weight          1276.32
 
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'
 'P'  'P'   0.1023   0.0942
 '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'
 'Pd'  'Pd'  -0.9988   1.0072
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            Tetragonal
_symmetry_space_group_name_H-M    I4(1)/acd
_symmetry_space_group_name_hall   '-I 4bd 2c'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y+1/2, z'
 'x, -y, -z+1/2'
 '-x+1/2, y, -z'
 '-y+1/4, -x+1/4, -z+1/4'
 'y+3/4, x+1/4, -z+1/4'
 'y+1/4, -x+1/4, z+3/4'
 '-y+1/4, x+3/4, z+1/4'
 'x+1/2, y+1/2, z+1/2'
 '-x+1/2, -y+1, z+1/2'
 'x+1/2, -y+1/2, -z+1'
 '-x+1, y+1/2, -z+1/2'
 '-y+3/4, -x+3/4, -z+3/4'
 'y+5/4, x+3/4, -z+3/4'
 'y+3/4, -x+3/4, z+5/4'
 '-y+3/4, x+5/4, z+3/4'
 '-x, -y, -z'
 'x, y-1/2, -z'
 '-x, y, z-1/2'
 'x-1/2, -y, z'
 'y-1/4, x-1/4, z-1/4'
 '-y-3/4, -x-1/4, z-1/4'
 '-y-1/4, x-1/4, -z-3/4'
 'y-1/4, -x-3/4, -z-1/4'
 '-x+1/2, -y+1/2, -z+1/2'
 'x+1/2, y, -z+1/2'
 '-x+1/2, y+1/2, z'
 'x, -y+1/2, z+1/2'
 'y+1/4, x+1/4, z+1/4'
 '-y-1/4, -x+1/4, z+1/4'
 '-y+1/4, x+1/4, -z-1/4'
 'y+1/4, -x-1/4, -z+1/4'
 
_cell_length_a                    33.788(6)
_cell_length_b                    33.788(6)
_cell_length_c                    22.014(7)
_cell_angle_alpha                 90.000
_cell_angle_beta                  90.000
_cell_angle_gamma                 90.000
_cell_volume                      25132(10)
_cell_formula_units_Z             16
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     13960
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Block
_exptl_crystal_colour             Yellow
_exptl_crystal_size_max           0.20
_exptl_crystal_size_mid           0.18
_exptl_crystal_size_min           0.12
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.349
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              10496
_exptl_absorpt_coefficient_mu     0.534
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9007
_exptl_absorpt_correction_T_max   0.9387
_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             63810
_diffrn_reflns_av_R_equivalents   0.2781
_diffrn_reflns_av_sigmaI/netI     0.1868
_diffrn_reflns_limit_h_min        -40
_diffrn_reflns_limit_h_max        40
_diffrn_reflns_limit_k_min        -40
_diffrn_reflns_limit_k_max        34
_diffrn_reflns_limit_l_min        -26
_diffrn_reflns_limit_l_max        26
_diffrn_reflns_theta_min          3.04
_diffrn_reflns_theta_max          25.02
_reflns_number_total              5531
_reflns_number_gt                 1784
_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)+(0.1041P)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     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          5531
_refine_ls_number_parameters      377
_refine_ls_number_restraints      1
_refine_ls_R_factor_all           0.2565
_refine_ls_R_factor_gt            0.0801
_refine_ls_wR_factor_ref          0.2391
_refine_ls_wR_factor_gt           0.1689
_refine_ls_goodness_of_fit_ref    0.920
_refine_ls_restrained_S_all       0.920
_refine_ls_shift/su_max           0.003
_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
Pd1 Pd 0.5000 0.0000 0.5000 0.0565(3) Uani 1 2 d S . .
Cl1 Cl 0.61018(10) -0.13982(10) 0.6250 0.0839(13) Uani 1 2 d S . .
P1 P 0.48199(9) 0.01866(8) 0.59928(12) 0.0627(8) Uani 1 1 d . . .
P2 P 0.55669(8) 0.04009(8) 0.50091(13) 0.0623(8) Uani 1 1 d . . .
N1 N 0.4607(3) -0.0594(2) 0.6135(4) 0.062(2) Uani 1 1 d . . .
O1 O 0.53124(12) -0.0951(2) 0.6133(3) 0.070(2) Uani 1 1 d D . .
O2 O 0.3993(2) -0.0563(3) 0.6987(4) 0.091(2) Uani 1 1 d . . .
H2 H 0.3764 -0.0466 0.6993 0.136 Uiso 1 1 calc R . .
O3 O 0.3668(3) -0.1126(3) 0.7017(4) 0.118(3) Uani 1 1 d . . .
C1 C 0.4347(3) 0.0448(3) 0.5951(5) 0.065(3) Uani 1 1 d . . .
C2 C 0.4244(4) 0.0649(3) 0.5436(6) 0.077(3) Uani 1 1 d . . .
H2A H 0.4421 0.0652 0.5101 0.092 Uiso 1 1 calc R . .
C3 C 0.3886(5) 0.0847(4) 0.5393(6) 0.090(4) Uani 1 1 d . . .
H3 H 0.3819 0.0984 0.5031 0.108 Uiso 1 1 calc R . .
C4 C 0.3632(4) 0.0844(4) 0.5867(8) 0.100(4) Uani 1 1 d . . .
H4 H 0.3385 0.0977 0.5836 0.120 Uiso 1 1 calc R . .
C5 C 0.3733(4) 0.0646(4) 0.6406(7) 0.096(4) Uani 1 1 d . . .
H5 H 0.3555 0.0647 0.6740 0.115 Uiso 1 1 calc R . .
C6 C 0.4086(4) 0.0451(3) 0.6451(5) 0.075(3) Uani 1 1 d . . .
H6 H 0.4156 0.0319 0.6817 0.091 Uiso 1 1 calc R . .
C7 C 0.5108(3) 0.0492(3) 0.6524(4) 0.063(3) Uani 1 1 d . . .
C8 C 0.4984(3) 0.0877(3) 0.6652(4) 0.067(3) Uani 1 1 d . . .
H8 H 0.4760 0.0988 0.6457 0.081 Uiso 1 1 calc R . .
C9 C 0.5201(5) 0.1090(3) 0.7074(5) 0.081(4) Uani 1 1 d . . .
H9 H 0.5116 0.1350 0.7174 0.097 Uiso 1 1 calc R . .
C10 C 0.5532(4) 0.0942(4) 0.7355(5) 0.079(4) Uani 1 1 d . . .
H10 H 0.5676 0.1099 0.7637 0.095 Uiso 1 1 calc R . .
C11 C 0.5646(4) 0.0578(4) 0.7226(5) 0.079(4) Uani 1 1 d . . .
H11 H 0.5872 0.0471 0.7423 0.095 Uiso 1 1 calc R . .
C12 C 0.5440(3) 0.0345(4) 0.6805(5) 0.072(3) Uani 1 1 d . . .
H12 H 0.5530 0.0086 0.6713 0.087 Uiso 1 1 calc R . .
C13 C 0.5990(4) 0.0184(3) 0.5397(5) 0.066(3) Uani 1 1 d . . .
C14 C 0.6359(4) 0.0341(4) 0.5316(6) 0.086(4) Uani 1 1 d . . .
H14 H 0.6399 0.0560 0.5053 0.104 Uiso 1 1 calc R . .
C15 C 0.6666(5) 0.0174(5) 0.5619(8) 0.127(6) Uani 1 1 d . . .
H15 H 0.6926 0.0275 0.5560 0.153 Uiso 1 1 calc R . .
C16 C 0.6608(6) -0.0140(6) 0.6015(10) 0.141(7) Uani 1 1 d . . .
H16 H 0.6827 -0.0242 0.6235 0.169 Uiso 1 1 calc R . .
C17 C 0.6242(5) -0.0308(4) 0.6095(7) 0.110(5) Uani 1 1 d . . .
H17 H 0.6204 -0.0525 0.6364 0.132 Uiso 1 1 calc R . .
C18 C 0.5927(4) -0.0150(4) 0.5767(6) 0.090(4) Uani 1 1 d . . .
H18 H 0.5672 -0.0266 0.5792 0.108 Uiso 1 1 calc R . .
C19 C 0.5484(4) 0.0893(3) 0.5322(5) 0.066(3) Uani 1 1 d . . .
C20 C 0.5756(4) 0.1070(4) 0.5728(5) 0.072(3) Uani 1 1 d . . .
H20 H 0.5977 0.0924 0.5870 0.086 Uiso 1 1 calc R . .
C21 C 0.5700(4) 0.1456(4) 0.5916(5) 0.083(4) Uani 1 1 d . . .
H21 H 0.5886 0.1577 0.6180 0.100 Uiso 1 1 calc R . .
C22 C 0.5375(6) 0.1663(4) 0.5721(6) 0.103(5) Uani 1 1 d . . .
H22 H 0.5333 0.1926 0.5861 0.124 Uiso 1 1 calc R . .
C23 C 0.5103(4) 0.1489(4) 0.5315(5) 0.088(4) Uani 1 1 d . . .
H23 H 0.4880 0.1635 0.5174 0.105 Uiso 1 1 calc R . .
C24 C 0.5164(4) 0.1107(4) 0.5124(5) 0.078(3) Uani 1 1 d . . .
H24 H 0.4981 0.0989 0.4851 0.093 Uiso 1 1 calc R . .
C25 C 0.4647(4) -0.0966(4) 0.6426(5) 0.071(3) Uani 1 1 d . . .
C26 C 0.5020(4) -0.1163(3) 0.6378(4) 0.061(3) Uani 1 1 d . . .
C27 C 0.5054(4) -0.1551(3) 0.6578(5) 0.077(4) Uani 1 1 d . . .
H27 H 0.5299 -0.1688 0.6539 0.092 Uiso 1 1 calc R . .
C28 C 0.4726(6) -0.1739(4) 0.6840(6) 0.099(5) Uani 1 1 d . . .
H28 H 0.4746 -0.2009 0.6959 0.119 Uiso 1 1 calc R . .
C29 C 0.4377(5) -0.1540(5) 0.6928(5) 0.087(4) Uani 1 1 d . . .
H29 H 0.4160 -0.1667 0.7121 0.104 Uiso 1 1 calc R . .
C30 C 0.4343(4) -0.1153(4) 0.6731(5) 0.079(4) Uani 1 1 d . . .
C31 C 0.3969(4) -0.0950(4) 0.6910(5) 0.075(3) Uani 1 1 d . . .
C32 C 0.4763(3) -0.0263(3) 0.6464(5) 0.069(3) Uani 1 1 d . . .
H32A H 0.5024 -0.0337 0.6634 0.083 Uiso 1 1 calc R . .
H32B H 0.4585 -0.0203 0.6809 0.083 Uiso 1 1 calc R . .
C33 C 0.4258(3) -0.0521(3) 0.5763(5) 0.072(3) Uani 1 1 d . . .
H33A H 0.4102 -0.0298 0.5931 0.087 Uiso 1 1 calc R . .
H33B H 0.4087 -0.0759 0.5754 0.087 Uiso 1 1 calc R . .
Cl2A Cl 0.3380(2) 0.0000 0.7500 0.114(3) Uani 0.606(9) 2 d SP A 1
Cl2B Cl 0.3199(5) 0.0285(6) 0.7899(10) 0.114(3) Uani 0.197(4) 1 d P A 2
H1 H 0.5534(13) -0.106(2) 0.613(4) 0.06(3) Uiso 1 1 d 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
Pd1 P2 2.346(3) 17_656 ?
Pd1 P2 2.346(3) . ?
Pd1 P1 2.355(3) . ?
Pd1 P1 2.355(3) 17_656 ?
P1 C1 1.828(11) . ?
P1 C7 1.839(11) . ?
P1 C32 1.851(11) . ?
P2 C13 1.819(12) . ?
P2 C19 1.820(11) . ?
P2 C33 1.846(11) 17_656 ?
N1 C25 1.418(13) . ?
N1 C32 1.432(12) . ?
N1 C33 1.456(12) . ?
O1 C26 1.333(13) . ?
O1 H1 0.8400(5) . ?
O2 C31 1.321(13) . ?
O2 H2 0.8400 . ?
O3 C31 1.203(13) . ?
C1 C2 1.367(15) . ?
C1 C6 1.409(14) . ?
C2 C3 1.386(16) . ?
C2 H2A 0.9500 . ?
C3 C4 1.350(17) . ?
C3 H3 0.9500 . ?
C4 C5 1.404(17) . ?
C4 H4 0.9500 . ?
C5 C6 1.367(15) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.372(14) . ?
C7 C8 1.393(13) . ?
C8 C9 1.386(15) . ?
C8 H8 0.9500 . ?
C9 C10 1.372(16) . ?
C9 H9 0.9500 . ?
C10 C11 1.320(15) . ?
C10 H10 0.9500 . ?
C11 C12 1.401(15) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.366(15) . ?
C13 C18 1.406(15) . ?
C14 C15 1.356(18) . ?
C14 H14 0.9500 . ?
C15 C16 1.39(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.37(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.392(17) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C24 1.374(15) . ?
C19 C20 1.414(14) . ?
C20 C21 1.380(15) . ?
C20 H20 0.9500 . ?
C21 C22 1.371(17) . ?
C21 H21 0.9500 . ?
C22 C23 1.412(18) . ?
C22 H22 0.9500 . ?
C23 C24 1.373(15) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C30 1.380(16) . ?
C25 C26 1.430(15) . ?
C26 C27 1.388(14) . ?
C27 C28 1.402(18) . ?
C27 H27 0.9500 . ?
C28 C29 1.372(19) . ?
C28 H28 0.9500 . ?
C29 C30 1.383(17) . ?
C29 H29 0.9500 . ?
C30 C31 1.492(17) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 P2 1.846(11) 17_656 ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
 
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
P2 Pd1 P2 180.0(2) 17_656 . ?
P2 Pd1 P1 87.22(10) 17_656 . ?
P2 Pd1 P1 92.78(10) . . ?
P2 Pd1 P1 92.78(10) 17_656 17_656 ?
P2 Pd1 P1 87.22(10) . 17_656 ?
P1 Pd1 P1 180.00(5) . 17_656 ?
C1 P1 C7 102.9(5) . . ?
C1 P1 C32 109.5(5) . . ?
C7 P1 C32 99.2(5) . . ?
C1 P1 Pd1 108.0(4) . . ?
C7 P1 Pd1 127.2(3) . . ?
C32 P1 Pd1 109.1(3) . . ?
C13 P2 C19 108.1(5) . . ?
C13 P2 C33 105.6(5) . 17_656 ?
C19 P2 C33 101.4(5) . 17_656 ?
C13 P2 Pd1 114.4(4) . . ?
C19 P2 Pd1 113.9(4) . . ?
C33 P2 Pd1 112.4(4) 17_656 . ?
C25 N1 C32 115.3(8) . . ?
C25 N1 C33 118.7(9) . . ?
C32 N1 C33 116.9(9) . . ?
C26 O1 H1 114(7) . . ?
C31 O2 H2 109.5 . . ?
C2 C1 C6 119.0(11) . . ?
C2 C1 P1 120.3(9) . . ?
C6 C1 P1 120.8(9) . . ?
C1 C2 C3 121.3(12) . . ?
C1 C2 H2A 119.4 . . ?
C3 C2 H2A 119.4 . . ?
C4 C3 C2 119.9(12) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C5 120.1(13) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C6 C5 C4 120.2(13) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C1 119.6(11) . . ?
C5 C6 H6 120.2 . . ?
C1 C6 H6 120.2 . . ?
C12 C7 C8 119.4(10) . . ?
C12 C7 P1 121.1(9) . . ?
C8 C7 P1 119.5(8) . . ?
C9 C8 C7 117.5(11) . . ?
C9 C8 H8 121.3 . . ?
C7 C8 H8 121.3 . . ?
C10 C9 C8 122.9(11) . . ?
C10 C9 H9 118.5 . . ?
C8 C9 H9 118.5 . . ?
C11 C10 C9 118.7(12) . . ?
C11 C10 H10 120.7 . . ?
C9 C10 H10 120.7 . . ?
C10 C11 C12 121.4(12) . . ?
C10 C11 H11 119.3 . . ?
C12 C11 H11 119.3 . . ?
C7 C12 C11 120.1(11) . . ?
C7 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C14 C13 C18 121.6(12) . . ?
C14 C13 P2 120.0(10) . . ?
C18 C13 P2 118.4(10) . . ?
C15 C14 C13 118.2(13) . . ?
C15 C14 H14 120.9 . . ?
C13 C14 H14 120.9 . . ?
C14 C15 C16 121.2(15) . . ?
C14 C15 H15 119.4 . . ?
C16 C15 H15 119.4 . . ?
C17 C16 C15 121.6(15) . . ?
C17 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?
C16 C17 C18 117.5(15) . . ?
C16 C17 H17 121.3 . . ?
C18 C17 H17 121.3 . . ?
C17 C18 C13 119.7(14) . . ?
C17 C18 H18 120.2 . . ?
C13 C18 H18 120.2 . . ?
C24 C19 C20 119.1(10) . . ?
C24 C19 P2 118.9(9) . . ?
C20 C19 P2 121.8(9) . . ?
C21 C20 C19 120.2(11) . . ?
C21 C20 H20 119.9 . . ?
C19 C20 H20 119.9 . . ?
C22 C21 C20 119.9(12) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C21 C22 C23 120.4(12) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 H22 119.8 . . ?
C24 C23 C22 119.2(13) . . ?
C24 C23 H23 120.4 . . ?
C22 C23 H23 120.4 . . ?
C23 C24 C19 121.2(12) . . ?
C23 C24 H24 119.4 . . ?
C19 C24 H24 119.4 . . ?
C30 C25 N1 123.7(13) . . ?
C30 C25 C26 118.6(12) . . ?
N1 C25 C26 117.7(11) . . ?
O1 C26 C27 125.0(12) . . ?
O1 C26 C25 115.6(10) . . ?
C27 C26 C25 119.4(12) . . ?
C26 C27 C28 119.6(13) . . ?
C26 C27 H27 120.2 . . ?
C28 C27 H27 120.2 . . ?
C29 C28 C27 121.0(13) . . ?
C29 C28 H28 119.5 . . ?
C27 C28 H28 119.5 . . ?
C28 C29 C30 119.4(14) . . ?
C28 C29 H29 120.3 . . ?
C30 C29 H29 120.3 . . ?
C25 C30 C29 121.7(13) . . ?
C25 C30 C31 123.2(13) . . ?
C29 C30 C31 115.0(14) . . ?
O3 C31 O2 121.0(13) . . ?
O3 C31 C30 122.8(14) . . ?
O2 C31 C30 116.1(12) . . ?
N1 C32 P1 113.2(7) . . ?
N1 C32 H32A 108.9 . . ?
P1 C32 H32A 108.9 . . ?
N1 C32 H32B 108.9 . . ?
P1 C32 H32B 108.9 . . ?
H32A C32 H32B 107.7 . . ?
N1 C33 P2 107.1(7) . 17_656 ?
N1 C33 H33A 110.3 . . ?
P2 C33 H33A 110.3 17_656 . ?
N1 C33 H33B 110.3 . . ?
P2 C33 H33B 110.3 17_656 . ?
H33A C33 H33B 108.5 . . ?
 
loop_
 _geom_hbond_atom_site_label_D
 _geom_hbond_atom_site_label_H
 _geom_hbond_atom_site_label_A
 _geom_hbond_distance_DH
 _geom_hbond_distance_HA
 _geom_hbond_distance_DA
 _geom_hbond_angle_DHA
 _geom_hbond_site_symmetry_A
O2 H2 Cl2A  0.84 2.32 3.029(10) 141.7 .
O1 H1 Cl1  0.84 2.240(13) 3.076(5) 173(9) .
 
_diffrn_measured_fraction_theta_max    0.994
_diffrn_reflns_theta_full              25.02
_diffrn_measured_fraction_theta_full   0.994
_refine_diff_density_max    0.570
_refine_diff_density_min   -0.332
_refine_diff_density_rms    0.082
