# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

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#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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#  fide research purposes only. It may contain copyright material
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data_pt
_audit_creation_date             2014-04-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C40 H38 N4 O6 P2 Pt'
_chemical_formula_sum            'C40 H38 N4 O6 P2 Pt'
_chemical_formula_weight         927.77
_chemical_melting_point          ?
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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.0856(13)
_cell_length_b                   13.6274(15)
_cell_length_c                   11.4059(13)
_cell_angle_alpha                90
_cell_angle_beta                 91.489(2)
_cell_angle_gamma                90
_cell_volume                     1877.9(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6416
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      2.25
_shelx_estimated_absorpt_T_max   0.698
_shelx_estimated_absorpt_T_min   0.613
_exptl_absorpt_coefficient_mu    3.874
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       ?
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16131
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.994
_diffrn_reflns_theta_min         2.253
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3507
_reflns_number_total             4907
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.442
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4907
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0225
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0327P)²+0.2885P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0645
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C20A-C19A = C20B-C19B
 1.51 with sigma of 0.01
3. Others
 Fixed Sof: C20A(0.5) H20A(0.5) H20B(0.5) H20C(0.5) C19A(0.5) H19A(0.5)
 H19B(0.5) C19B(0.5) H19C(0.5) H19D(0.5) C20B(0.5) H20D(0.5) H20E(0.5) H20F(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C19A(H19A,H19B), C19B(H19C,H19D)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C16(H16)
4.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C20A(H20A,H20B,H20C), C20B(H20D,H20E,H20F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.5000 0.5000 0.5000 0.02718(5) Uani 1 2 d S T P . .
P1 P 0.29058(7) 0.36101(7) 0.12188(7) 0.0485(2) Uani 1 1 d . . . . .
O1 O 0.1851(2) 0.4051(2) 0.0875(2) 0.0759(9) Uani 1 1 d . . . . .
O2 O 0.2839(2) 0.24804(18) 0.1486(2) 0.0622(7) Uani 1 1 d . . . . .
O3 O 0.3800(2) 0.3709(2) 0.0252(2) 0.0738(8) Uani 1 1 d . . . . .
N1 N 0.47013(18) 0.60427(17) 0.62074(18) 0.0335(5) Uani 1 1 d . . . . .
N2 N 0.3542(2) 0.52743(18) 0.4162(2) 0.0311(5) Uani 1 1 d . . . . .
C1 C 0.3753(2) 0.6600(2) 0.6260(2) 0.0392(7) Uani 1 1 d . . . . .
C2 C 0.3826(3) 0.7252(3) 0.7246(3) 0.0546(9) Uani 1 1 d . . . . .
H2 H 0.3295 0.7705 0.7465 0.066 Uiso 1 1 calc R . . . .
C3 C 0.2841(2) 0.6547(2) 0.5492(3) 0.0379(7) Uani 1 1 d . . . . .
C4 C 0.1858(3) 0.7171(3) 0.5744(3) 0.0478(8) Uani 1 1 d . . . . .
C5 C 0.1102(3) 0.6848(3) 0.6562(4) 0.0635(10) Uani 1 1 d . . . . .
H5 H 0.1231 0.6271 0.6978 0.076 Uiso 1 1 calc R . . . .
C6 C 0.0148(3) 0.7401(4) 0.6751(4) 0.0883(16) Uani 1 1 d . . . . .
H6 H -0.0363 0.7190 0.7293 0.106 Uiso 1 1 calc R . . . .
C7 C -0.0034(4) 0.8250(4) 0.6138(5) 0.0904(18) Uani 1 1 d . . . . .
H7 H -0.0673 0.8612 0.6261 0.108 Uiso 1 1 calc R . . . .
C8 C 0.0703(4) 0.8568(4) 0.5360(4) 0.0902(16) Uani 1 1 d . . . . .
H8 H 0.0574 0.9150 0.4954 0.108 Uiso 1 1 calc R . . . .
C9 C 0.1657(3) 0.8027(3) 0.5162(4) 0.0671(11) Uani 1 1 d . . . . .
H9 H 0.2164 0.8254 0.4625 0.081 Uiso 1 1 calc R . . . .
C10 C 0.2762(2) 0.5942(2) 0.4521(2) 0.0342(6) Uani 1 1 d . . . . .
C11 C 0.1816(2) 0.5907(2) 0.3729(3) 0.0424(7) Uani 1 1 d . . . . .
H11 H 0.1177 0.6283 0.3782 0.051 Uiso 1 1 calc R . . . .
C12 C 0.2020(3) 0.5244(3) 0.2911(3) 0.0436(8) Uani 1 1 d . . . . .
H12 H 0.1552 0.5079 0.2281 0.052 Uiso 1 1 calc R . . . .
C13 C 0.3098(3) 0.4821(2) 0.3170(3) 0.0339(6) Uani 1 1 d . . . . .
C14 C 0.3605(2) 0.4076(2) 0.2539(2) 0.0379(6) Uani 1 1 d . . . . .
C15 C 0.4634(2) 0.3670(2) 0.2842(2) 0.0379(6) Uani 1 1 d . . . . .
C16 C 0.5201(3) 0.2914(3) 0.2208(3) 0.0530(9) Uani 1 1 d . . . . .
H16 H 0.4935 0.2596 0.1536 0.064 Uiso 1 1 calc R . . . .
C17 C 0.2435(4) 0.1815(4) 0.0576(4) 0.0873(16) Uani 1 1 d . . . . .
H17A H 0.2202 0.2196 -0.0105 0.105 Uiso 1 1 calc R . . . .
H17B H 0.3039 0.1394 0.0344 0.105 Uiso 1 1 calc R . . . .
C18 C 0.1555(5) 0.1229(4) 0.0919(5) 0.118(2) Uani 1 1 d . . . . .
H18A H 0.1381 0.0760 0.0314 0.177 Uiso 1 1 calc GR . . . .
H18B H 0.0920 0.1634 0.1050 0.177 Uiso 1 1 calc GR . . . .
H18C H 0.1758 0.0889 0.1630 0.177 Uiso 1 1 calc GR . . . .
C20A C 0.368(3) 0.4684(11) -0.1540(17) 0.183(12) Uani 0.5 1 d D . . A 1
H20A H 0.3306 0.5189 -0.1112 0.274 Uiso 0.5 1 calc GR . . A 1
H20B H 0.3366 0.4650 -0.2323 0.274 Uiso 0.5 1 calc GR . . A 1
H20C H 0.4450 0.4834 -0.1570 0.274 Uiso 0.5 1 calc GR . . A 1
C19A C 0.3530(10) 0.3752(9) -0.0962(8) 0.098(4) Uani 0.5 1 d D . . A 1
H19A H 0.2762 0.3558 -0.1071 0.118 Uiso 0.5 1 calc R . . A 1
H19B H 0.3976 0.3269 -0.1357 0.118 Uiso 0.5 1 calc R . . A 1
C19B C 0.3747(15) 0.4551(13) -0.0568(12) 0.147(6) Uani 0.5 1 d D . . A 2
H19C H 0.2992 0.4782 -0.0675 0.177 Uiso 0.5 1 calc R . . A 2
H19D H 0.4204 0.5089 -0.0279 0.177 Uiso 0.5 1 calc R . . A 2
C20B C 0.416(3) 0.4168(13) -0.1660(17) 0.217(16) Uani 0.5 1 d D . . A 2
H20D H 0.4861 0.3848 -0.1510 0.326 Uiso 0.5 1 calc GR . . A 2
H20E H 0.4261 0.4697 -0.2203 0.326 Uiso 0.5 1 calc GR . . A 2
H20F H 0.3644 0.3704 -0.1988 0.326 Uiso 0.5 1 calc GR . . A 2


_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
Pt1 N1 2.018(2) . ?
Pt1 N1 2.018(2) 3_666 ?
Pt1 N2 2.018(2) . ?
Pt1 N2 2.018(2) 3_666 ?
P1 O1 1.454(2) . ?
P1 O2 1.572(3) . ?
P1 O3 1.569(3) . ?
P1 C14 1.821(3) . ?
O2 C17 1.453(4) . ?
O3 C19A 1.416(9) . ?
O3 C19B 1.482(16) . ?
N1 C1 1.378(3) . ?
N1 C15 1.389(3) 3_666 ?
N2 C10 1.379(4) . ?
N2 C13 1.384(4) . ?
C1 C2 1.434(4) . ?
C1 C3 1.392(4) . ?
C2 C16 1.336(4) 3_666 ?
C3 C4 1.495(4) . ?
C3 C10 1.382(4) . ?
C4 C5 1.393(5) . ?
C4 C9 1.362(5) . ?
C5 C6 1.399(5) . ?
C6 C7 1.366(7) . ?
C7 C8 1.345(7) . ?
C8 C9 1.392(5) . ?
C10 C11 1.439(4) . ?
C11 C12 1.328(4) . ?
C12 C13 1.448(4) . ?
C13 C14 1.396(4) . ?
C14 C15 1.396(4) . ?
C15 N1 1.389(3) 3_666 ?
C15 C16 1.443(4) . ?
C16 C2 1.336(4) 3_666 ?
C17 C18 1.394(7) . ?
C20A C19A 1.444(9) . ?
C19B C20B 1.452(9) . ?

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 Pt1 N1 180.0 . 3_666 ?
N1 Pt1 N2 91.34(9) . . ?
N1 Pt1 N2 88.66(9) . 3_666 ?
N1 Pt1 N2 91.34(9) 3_666 3_666 ?
N1 Pt1 N2 88.66(9) 3_666 . ?
N2 Pt1 N2 180.00(12) . 3_666 ?
O1 P1 O2 114.07(17) . . ?
O1 P1 O3 112.96(17) . . ?
O1 P1 C14 117.59(14) . . ?
O2 P1 C14 101.90(13) . . ?
O3 P1 O2 105.07(16) . . ?
O3 P1 C14 103.77(14) . . ?
C17 O2 P1 119.4(3) . . ?
C19A O3 P1 123.1(5) . . ?
C19B O3 P1 119.4(7) . . ?
C1 N1 Pt1 125.57(17) . . ?
C1 N1 C15 106.0(2) . 3_666 ?
C15 N1 Pt1 128.37(18) 3_666 . ?
C10 N2 Pt1 125.18(18) . . ?
C10 N2 C13 106.5(2) . . ?
C13 N2 Pt1 128.3(2) . . ?
N1 C1 C2 109.9(2) . . ?
N1 C1 C3 126.2(3) . . ?
C3 C1 C2 123.9(3) . . ?
C16 C2 C1 107.3(3) 3_666 . ?
C1 C3 C4 118.0(3) . . ?
C10 C3 C1 124.9(3) . . ?
C10 C3 C4 117.1(3) . . ?
C5 C4 C3 119.2(3) . . ?
C9 C4 C3 121.7(3) . . ?
C9 C4 C5 119.0(3) . . ?
C4 C5 C6 119.4(4) . . ?
C7 C6 C5 119.9(5) . . ?
C8 C7 C6 120.6(4) . . ?
C7 C8 C9 120.2(5) . . ?
C4 C9 C8 120.8(5) . . ?
N2 C10 C3 126.7(2) . . ?
N2 C10 C11 109.3(2) . . ?
C3 C10 C11 124.0(3) . . ?
C12 C11 C10 107.7(3) . . ?
C11 C12 C13 108.0(3) . . ?
N2 C13 C12 108.5(3) . . ?
N2 C13 C14 125.5(3) . . ?
C14 C13 C12 126.0(3) . . ?
C13 C14 P1 118.7(2) . . ?
C13 C14 C15 124.0(3) . . ?
C15 C14 P1 117.3(2) . . ?
N1 C15 C14 125.2(3) 3_666 . ?
N1 C15 C16 108.6(2) 3_666 . ?
C14 C15 C16 126.2(3) . . ?
C2 C16 C15 108.1(3) 3_666 . ?
C18 C17 O2 113.6(4) . . ?
O3 C19A C20A 117.1(12) . . ?
C20B C19B O3 104.6(15) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pt1 N1 C1 C2 179.0(2) . . . . ?
Pt1 N1 C1 C3 -0.4(5) . . . . ?
Pt1 N2 C10 C3 1.2(4) . . . . ?
Pt1 N2 C10 C11 -177.9(2) . . . . ?
Pt1 N2 C13 C12 178.4(2) . . . . ?
Pt1 N2 C13 C14 -1.0(4) . . . . ?
P1 O2 C17 C18 -125.4(5) . . . . ?
P1 O3 C19A C20A 108.9(17) . . . . ?
P1 O3 C19B C20B -147.1(18) . . . . ?
P1 C14 C15 N1 177.7(2) . . . 3_666 ?
P1 C14 C15 C16 0.0(5) . . . . ?
O1 P1 O2 C17 59.0(3) . . . . ?
O1 P1 O3 C19A -29.5(6) . . . . ?
O1 P1 O3 C19B 28.4(8) . . . . ?
O1 P1 C14 C13 0.8(3) . . . . ?
O1 P1 C14 C15 -178.0(3) . . . . ?
O2 P1 O3 C19A 95.5(6) . . . . ?
O2 P1 O3 C19B 153.4(8) . . . . ?
O2 P1 C14 C13 -124.7(3) . . . . ?
O2 P1 C14 C15 56.5(3) . . . . ?
O3 P1 O2 C17 -65.3(3) . . . . ?
O3 P1 C14 C13 126.3(3) . . . . ?
O3 P1 C14 C15 -52.5(3) . . . . ?
N1 C1 C2 C16 -0.7(4) . . . 3_666 ?
N1 C1 C3 C4 176.1(3) . . . . ?
N1 C1 C3 C10 -2.3(5) . . . . ?
N1 C15 C16 C2 0.0(4) 3_666 . . 3_666 ?
N2 C10 C11 C12 -0.4(4) . . . . ?
N2 C13 C14 P1 -177.5(2) . . . . ?
N2 C13 C14 C15 1.2(5) . . . . ?
C1 C3 C4 C5 -81.6(4) . . . . ?
C1 C3 C4 C9 101.0(4) . . . . ?
C1 C3 C10 N2 1.9(5) . . . . ?
C1 C3 C10 C11 -179.2(3) . . . . ?
C2 C1 C3 C4 -3.2(5) . . . . ?
C2 C1 C3 C10 178.4(3) . . . . ?
C3 C1 C2 C16 178.7(3) . . . 3_666 ?
C3 C4 C5 C6 -176.3(3) . . . . ?
C3 C4 C9 C8 176.2(3) . . . . ?
C3 C10 C11 C12 -179.4(3) . . . . ?
C4 C3 C10 N2 -176.5(3) . . . . ?
C4 C3 C10 C11 2.4(5) . . . . ?
C4 C5 C6 C7 -0.2(6) . . . . ?
C5 C4 C9 C8 -1.2(6) . . . . ?
C5 C6 C7 C8 -0.6(7) . . . . ?
C6 C7 C8 C9 0.6(7) . . . . ?
C7 C8 C9 C4 0.3(6) . . . . ?
C9 C4 C5 C6 1.2(5) . . . . ?
C10 N2 C13 C12 1.0(3) . . . . ?
C10 N2 C13 C14 -178.3(3) . . . . ?
C10 C3 C4 C5 96.9(4) . . . . ?
C10 C3 C4 C9 -80.4(4) . . . . ?
C10 C11 C12 C13 1.0(4) . . . . ?
C11 C12 C13 N2 -1.3(4) . . . . ?
C11 C12 C13 C14 178.0(3) . . . . ?
C12 C13 C14 P1 3.3(4) . . . . ?
C12 C13 C14 C15 -178.0(3) . . . . ?
C13 N2 C10 C3 178.6(3) . . . . ?
C13 N2 C10 C11 -0.4(3) . . . . ?
C13 C14 C15 N1 -1.0(5) . . . 3_666 ?
C13 C14 C15 C16 -178.8(3) . . . . ?
C14 P1 O2 C17 -173.3(3) . . . . ?
C14 P1 O3 C19A -157.9(6) . . . . ?
C14 P1 O3 C19B -100.0(8) . . . . ?
C14 C15 C16 C2 178.0(3) . . . 3_666 ?
C15 N1 C1 C2 0.7(3) 3_666 . . . ?
C15 N1 C1 C3 -178.7(3) 3_666 . . . ?
C19A O3 C19B C20B -37.2(19) . . . . ?
C19B O3 C19A C20A 7(2) . . . . ?

_database_code_depnum_ccdc_archive 'CCDC 998787'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_ni
_audit_creation_date             2014-04-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '2(C40 H38 N4 Ni O6 P2), C6 H14'
_chemical_formula_sum            'C86 H90 N8 Ni2 O12 P4'
_chemical_formula_weight         1668.95
_chemical_melting_point          ?
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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.151(5)
_cell_length_b                   13.187(5)
_cell_length_c                   13.280(5)
_cell_angle_alpha                91.426(6)
_cell_angle_beta                 110.824(5)
_cell_angle_gamma                107.172(5)
_cell_volume                     2034.8(13)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    4070
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.09
_cell_measurement_theta_min      2.28
_shelx_estimated_absorpt_T_max   0.953
_shelx_estimated_absorpt_T_min   0.931
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       ?
_exptl_crystal_F_000             874
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0845
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            7866
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.017
_diffrn_reflns_theta_min         1.634
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5094
_reflns_number_total             7866
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.820
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         7866
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.1268
_refine_ls_R_factor_gt           0.0806
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1488P)²+0.0306P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2270
_refine_ls_wR_factor_ref         0.2460
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C25A, C26A, C27A, C28A, C29A, C30A, C25B, C26B, C27B, C28B, C29B, C30B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C25A) = Uanis(C25B)
4. Others
 Sof(C25B)=Sof(C26B)=Sof(H26B)=Sof(C27B)=Sof(H27B)=Sof(C28B)=Sof(H28B)=
 Sof(C29B)=Sof(H29B)=Sof(C30B)=Sof(H30B)=1-FVAR(1)
 Sof(C25A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28A)=
 Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C23(H23A,H23B), C31(H31A,H31B), C33(H33A,H33B), C42(H42A,
 H42B), C43(H43A,H43B)
5.b Me refined with riding coordinates:
 C41(H41A,H41B,H41C)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C13(H13), C14(H14), C18(H18), C19(H19), C26A(H26A),
 C27A(H27A), C28A(H28A), C29A(H29A), C30A(H30A), C26B(H26B), C27B(H27B),
 C28B(H28B), C29B(H29B), C30B(H30B), C36(H36), C37(H37), C38(H38), C39(H39),
 C40(H40), C17(H17)
5.d Fitted hexagon refined as free rotating group:
 C25A(C26A,C27A,C28A,C29A,C30A), C25B(C26B,C27B,C28B,C29B,C30B)
5.e Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C), C34(H34A,H34B,
 H34C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.00902(5) 0.73812(5) 0.23272(5) 0.0279(2) Uani 1 1 d . . . . .
P1 P 0.37820(12) 0.69113(12) 0.50235(12) 0.0363(4) Uani 1 1 d . . . . .
P2 P -0.38894(13) 0.78030(15) 0.14623(14) 0.0461(4) Uani 1 1 d . . . . .
O1 O 0.4582(3) 0.7921(3) 0.5704(3) 0.0478(11) Uani 1 1 d . . . . .
O2 O 0.3246(3) 0.6033(3) 0.5633(3) 0.0446(10) Uani 1 1 d . . . . .
O3 O 0.4326(3) 0.6219(3) 0.4529(3) 0.0401(10) Uani 1 1 d . . . . .
O4 O -0.4812(3) 0.6817(4) 0.1370(4) 0.0562(13) Uani 1 1 d . . . . .
O5 O -0.4196(3) 0.8427(4) 0.0463(4) 0.0530(12) Uani 1 1 d . . . . .
O6 O -0.3543(4) 0.8655(4) 0.2451(4) 0.0575(13) Uani 1 1 d . . . . .
N1 N 0.0653(4) 0.6198(3) 0.2561(3) 0.0290(10) Uani 1 1 d . . . . .
N2 N -0.1445(4) 0.6428(4) 0.1602(4) 0.0332(11) Uani 1 1 d . . . . .
N3 N -0.0471(3) 0.8557(3) 0.2061(3) 0.0290(10) Uani 1 1 d . . . . .
N4 N 0.1629(3) 0.8342(3) 0.3021(3) 0.0262(9) Uani 1 1 d . . . . .
C1 C 0.2576(4) 0.7093(4) 0.3943(4) 0.0300(12) Uani 1 1 d . . . . .
C2 C 0.1670(4) 0.6178(4) 0.3321(4) 0.0318(12) Uani 1 1 d . . . . .
C3 C 0.1731(5) 0.5109(4) 0.3268(5) 0.0414(15) Uani 1 1 d . . . . .
H3 H 0.2333 0.4878 0.3730 0.050 Uiso 1 1 calc R . . . .
C4 C 0.2047(4) 0.9401(4) 0.2863(4) 0.0280(11) Uani 1 1 d . . . . .
C5 C 0.0086(5) 0.5155(4) 0.2010(4) 0.0336(13) Uani 1 1 d . . . . .
C6 C -0.1039(5) 0.4789(4) 0.1249(4) 0.0344(13) Uani 1 1 d . . . . .
C7 C -0.1766(5) 0.5383(5) 0.1101(4) 0.0371(14) Uani 1 1 d . . . . .
C8 C -0.2996(5) 0.4970(5) 0.0568(5) 0.0535(19) Uani 1 1 d . . . . .
H8 H -0.3433 0.4289 0.0133 0.064 Uiso 1 1 calc R . . . .
C9 C 0.0780(5) 0.4500(5) 0.2445(5) 0.0440(15) Uani 1 1 d . . . . .
H9 H 0.0600 0.3763 0.2196 0.053 Uiso 1 1 calc R . . . .
C10 C -0.2462(5) 0.6642(5) 0.1428(5) 0.0395(14) Uani 1 1 d . . . . .
C11 C -0.2515(4) 0.7653(5) 0.1648(4) 0.0365(13) Uani 1 1 d . . . . .
C12 C -0.1573(4) 0.8566(4) 0.1864(4) 0.0336(13) Uani 1 1 d . . . . .
C13 C -0.1599(5) 0.9638(5) 0.1759(5) 0.0424(15) Uani 1 1 d . . . . .
H13 H -0.2244 0.9869 0.1657 0.051 Uiso 1 1 calc R . . . .
C14 C -0.0549(5) 1.0263(5) 0.1829(5) 0.0392(14) Uani 1 1 d . . . . .
H14 H -0.0329 1.0999 0.1744 0.047 Uiso 1 1 calc R . . . .
C15 C 0.0160(4) 0.9599(4) 0.2058(4) 0.0290(12) Uani 1 1 d . . . . .
C16 C 0.1351(4) 0.9996(4) 0.2343(4) 0.0274(11) Uani 1 1 d . . . . .
C18 C 0.3271(4) 0.9813(4) 0.3408(4) 0.0321(12) Uani 1 1 d . . . . .
H18 H 0.3765 1.0498 0.3392 0.038 Uiso 1 1 calc R . . . .
C19 C 0.3584(4) 0.9031(4) 0.3949(4) 0.0321(12) Uani 1 1 d . . . . .
H19 H 0.4342 0.9082 0.4417 0.039 Uiso 1 1 calc R . . . .
C20 C 0.2579(4) 0.8116(4) 0.3697(4) 0.0302(12) Uani 1 1 d . . . . .
C21 C 0.2652(7) 0.6280(7) 0.6289(7) 0.073(2) Uani 1 1 d . . . . .
H21A H 0.3204 0.6557 0.7047 0.087 Uiso 1 1 calc R . . . .
H21B H 0.2318 0.6844 0.6000 0.087 Uiso 1 1 calc R . . . .
C22 C 0.1770(12) 0.5353(11) 0.6275(11) 0.159(6) Uani 1 1 d . . . . .
H22A H 0.1426 0.4915 0.5556 0.239 Uiso 1 1 calc GR . . . .
H22B H 0.1179 0.5562 0.6430 0.239 Uiso 1 1 calc GR . . . .
H22C H 0.2093 0.4936 0.6830 0.239 Uiso 1 1 calc GR . . . .
C23 C 0.4941(6) 0.6650(6) 0.3851(6) 0.0567(18) Uani 1 1 d . . . . .
H23A H 0.5404 0.7412 0.4137 0.068 Uiso 1 1 calc R . . . .
H23B H 0.4390 0.6612 0.3102 0.068 Uiso 1 1 calc R . . . .
C24 C 0.5713(7) 0.6015(8) 0.3838(8) 0.080(3) Uani 1 1 d . . . . .
H24A H 0.6192 0.6349 0.3437 0.120 Uiso 1 1 calc GR . . . .
H24B H 0.5245 0.5280 0.3481 0.120 Uiso 1 1 calc GR . . . .
H24C H 0.6207 0.6001 0.4587 0.120 Uiso 1 1 calc GR . . . .
C25A C -0.1399(6) 0.3593(5) 0.0748(6) 0.029(2) Uani 0.548(7) 1 d . U P A 1
C26A C -0.0844(6) 0.3292(5) 0.0134(6) 0.039(3) Uani 0.548(7) 1 d G U P A 1
H26A H -0.0207 0.3806 0.0056 0.047 Uiso 0.548(7) 1 calc R . P A 1
C27A C -0.1222(7) 0.2238(6) -0.0366(6) 0.048(3) Uani 0.548(7) 1 d G U P A 1
H27A H -0.0843 0.2032 -0.0786 0.058 Uiso 0.548(7) 1 calc R . P A 1
C28A C -0.2154(7) 0.1485(4) -0.0252(7) 0.048(3) Uani 0.548(7) 1 d G U P A 1
H28A H -0.2412 0.0764 -0.0594 0.057 Uiso 0.548(7) 1 calc R . P A 1
C29A C -0.2709(6) 0.1786(6) 0.0362(8) 0.047(3) Uani 0.548(7) 1 d G U P A 1
H29A H -0.3346 0.1272 0.0440 0.056 Uiso 0.548(7) 1 calc R . P A 1
C30A C -0.2331(6) 0.2840(7) 0.0862(7) 0.036(3) Uani 0.548(7) 1 d G U P A 1
H30A H -0.2710 0.3046 0.1281 0.043 Uiso 0.548(7) 1 calc R . P A 1
C25B C -0.1635(9) 0.3754(8) 0.0616(8) 0.029(2) Uani 0.452(7) 1 d . U P A 2
C26B C -0.1956(10) 0.3594(7) -0.0508(8) 0.058(4) Uani 0.452(7) 1 d G U P A 2
H26B H -0.1824 0.4192 -0.0885 0.069 Uiso 0.452(7) 1 calc R . P A 2
C27B C -0.2470(10) 0.2560(9) -0.1080(8) 0.080(6) Uani 0.452(7) 1 d G U P A 2
H27B H -0.2689 0.2451 -0.1847 0.096 Uiso 0.452(7) 1 calc R . P A 2
C28B C -0.2662(10) 0.1686(7) -0.0528(12) 0.079(6) Uani 0.452(7) 1 d G U P A 2
H28B H -0.3013 0.0979 -0.0919 0.095 Uiso 0.452(7) 1 calc R . P A 2
C29B C -0.2341(11) 0.1845(9) 0.0595(12) 0.089(8) Uani 0.452(7) 1 d G U P A 2
H29B H -0.2473 0.1248 0.0972 0.107 Uiso 0.452(7) 1 calc R . P A 2
C30B C -0.1827(11) 0.2879(11) 0.1167(8) 0.059(5) Uani 0.452(7) 1 d G U P A 2
H30B H -0.1608 0.2988 0.1935 0.071 Uiso 0.452(7) 1 calc R . P A 2
C31 C -0.4571(7) 0.7825(6) -0.0636(6) 0.068(2) Uani 1 1 d . . . . .
H31A H -0.4021 0.7450 -0.0638 0.082 Uiso 1 1 calc R . . . .
H31B H -0.5338 0.7279 -0.0825 0.082 Uiso 1 1 calc R . . . .
C32 C -0.4624(8) 0.8542(8) -0.1416(7) 0.090(3) Uani 1 1 d . . . . .
H32A H -0.4841 0.8145 -0.2135 0.134 Uiso 1 1 calc GR . . . .
H32B H -0.3870 0.9094 -0.1214 0.134 Uiso 1 1 calc GR . . . .
H32C H -0.5200 0.8883 -0.1439 0.134 Uiso 1 1 calc GR . . . .
C33 C -0.4305(6) 0.9203(6) 0.2558(7) 0.065(2) Uani 1 1 d . . . . .
H33A H -0.4944 0.8704 0.2709 0.078 Uiso 1 1 calc R . . . .
H33B H -0.4635 0.9485 0.1875 0.078 Uiso 1 1 calc R . . . .
C34 C -0.3627(8) 1.0096(8) 0.3469(7) 0.087(3) Uani 1 1 d . . . . .
H34A H -0.3021 1.0604 0.3295 0.131 Uiso 1 1 calc GR . . . .
H34B H -0.3277 0.9812 0.4133 0.131 Uiso 1 1 calc GR . . . .
H34C H -0.4134 1.0464 0.3582 0.131 Uiso 1 1 calc GR . . . .
C35 C 0.1861(4) 1.1115(4) 0.2172(4) 0.0298(12) Uani 1 1 d . . . . .
C36 C 0.1510(5) 1.1391(5) 0.1132(5) 0.0401(14) Uani 1 1 d . . . . .
H36 H 0.0982 1.0854 0.0536 0.048 Uiso 1 1 calc R . . . .
C37 C 0.1916(6) 1.2436(5) 0.0947(5) 0.0479(16) Uani 1 1 d . . . . .
H37 H 0.1665 1.2610 0.0229 0.057 Uiso 1 1 calc R . . . .
C38 C 0.2687(6) 1.3229(5) 0.1809(6) 0.0517(17) Uani 1 1 d . . . . .
H38 H 0.2964 1.3947 0.1687 0.062 Uiso 1 1 calc R . . . .
C39 C 0.3052(5) 1.2960(5) 0.2855(5) 0.0435(15) Uani 1 1 d . . . . .
H39 H 0.3593 1.3494 0.3449 0.052 Uiso 1 1 calc R . . . .
C40 C 0.2633(5) 1.1925(4) 0.3029(5) 0.0354(13) Uani 1 1 d . . . . .
H40 H 0.2873 1.1757 0.3750 0.043 Uiso 1 1 calc R . . . .
C17 C -0.3413(5) 0.5714(5) 0.0793(6) 0.059(2) Uani 1 1 d . . . . .
H17 H -0.4204 0.5643 0.0572 0.070 Uiso 1 1 calc R . . . .
C41 C -0.025(2) 0.7486(13) 0.537(3) 0.311(18) Uani 1 1 d . . . . .
H41A H -0.0856 0.6850 0.5391 0.467 Uiso 1 1 calc R . . . .
H41B H 0.0391 0.7688 0.6084 0.467 Uiso 1 1 calc R . . . .
H41C H 0.0027 0.7325 0.4812 0.467 Uiso 1 1 calc R . . . .
C42 C -0.0745(15) 0.8445(19) 0.5101(13) 0.214(12) Uani 1 1 d . . . . .
H42A H -0.1395 0.8233 0.4385 0.257 Uiso 1 1 calc R . . . .
H42B H -0.1049 0.8584 0.5655 0.257 Uiso 1 1 calc R . . . .
C43 C 0.0119(17) 0.9443(15) 0.5072(13) 0.188(11) Uani 1 1 d . . . . .
H43A H 0.0360 0.9286 0.4476 0.226 Uiso 1 1 calc R . . . .
H43B H 0.0798 0.9572 0.5758 0.226 Uiso 1 1 calc R . . . .


_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
Ni1 N1 1.903(4) . ?
Ni1 N2 1.909(4) . ?
Ni1 N3 1.895(4) . ?
Ni1 N4 1.911(4) . ?
P1 O1 1.461(4) . ?
P1 O2 1.569(5) . ?
P1 O3 1.571(4) . ?
P1 C1 1.804(5) . ?
P2 O4 1.460(5) . ?
P2 O5 1.572(5) . ?
P2 O6 1.547(5) . ?
P2 C11 1.807(6) . ?
O2 C21 1.448(9) . ?
O3 C23 1.434(8) . ?
O5 C31 1.484(9) . ?
O6 C33 1.439(8) . ?
N1 C2 1.368(7) . ?
N1 C5 1.393(6) . ?
N2 C7 1.389(7) . ?
N2 C10 1.388(8) . ?
N3 C12 1.382(7) . ?
N3 C15 1.381(6) . ?
N4 C4 1.393(7) . ?
N4 C20 1.376(7) . ?
C1 C2 1.400(7) . ?
C1 C20 1.395(8) . ?
C2 C3 1.437(7) . ?
C3 H3 0.9500 . ?
C3 C9 1.340(8) . ?
C4 C16 1.390(8) . ?
C4 C18 1.430(7) . ?
C5 C6 1.391(7) . ?
C5 C9 1.423(8) . ?
C6 C7 1.372(9) . ?
C6 C25A 1.561(8) . ?
C6 C25B 1.424(9) . ?
C7 C8 1.436(8) . ?
C8 H8 0.9500 . ?
C8 C17 1.331(10) . ?
C9 H9 0.9500 . ?
C10 C11 1.384(9) . ?
C10 C17 1.438(8) . ?
C11 C12 1.384(8) . ?
C12 C13 1.432(8) . ?
C13 H13 0.9500 . ?
C13 C14 1.352(8) . ?
C14 H14 0.9500 . ?
C14 C15 1.423(8) . ?
C15 C16 1.398(7) . ?
C16 C35 1.489(7) . ?
C18 H18 0.9500 . ?
C18 C19 1.351(8) . ?
C19 H19 0.9500 . ?
C19 C20 1.429(7) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.410(13) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.499(10) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25A C26A 1.3900 . ?
C25A C30A 1.3900 . ?
C26A H26A 0.9500 . ?
C26A C27A 1.3900 . ?
C27A H27A 0.9500 . ?
C27A C28A 1.3900 . ?
C28A H28A 0.9500 . ?
C28A C29A 1.3900 . ?
C29A H29A 0.9500 . ?
C29A C30A 1.3900 . ?
C30A H30A 0.9500 . ?
C25B C26B 1.3900 . ?
C25B C30B 1.3900 . ?
C26B H26B 0.9500 . ?
C26B C27B 1.3900 . ?
C27B H27B 0.9500 . ?
C27B C28B 1.3900 . ?
C28B H28B 0.9500 . ?
C28B C29B 1.3900 . ?
C29B H29B 0.9500 . ?
C29B C30B 1.3900 . ?
C30B H30B 0.9500 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.418(11) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.479(11) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.387(8) . ?
C35 C40 1.394(7) . ?
C36 H36 0.9500 . ?
C36 C37 1.386(8) . ?
C37 H37 0.9500 . ?
C37 C38 1.386(8) . ?
C38 H38 0.9500 . ?
C38 C39 1.392(9) . ?
C39 H39 0.9500 . ?
C39 C40 1.371(8) . ?
C40 H40 0.9500 . ?
C17 H17 0.9500 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C41 C42 1.58(3) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C42 C43 1.47(2) . ?
C43 C43 1.59(4) 2_576 ?
C43 H43A 0.9900 . ?
C43 H43B 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
N1 Ni1 N2 90.62(19) . . ?
N1 Ni1 N4 89.65(17) . . ?
N2 Ni1 N4 178.66(19) . . ?
N3 Ni1 N1 178.67(19) . . ?
N3 Ni1 N2 89.19(19) . . ?
N3 Ni1 N4 90.52(17) . . ?
O1 P1 O2 115.7(3) . . ?
O1 P1 O3 115.7(3) . . ?
O1 P1 C1 112.5(2) . . ?
O2 P1 O3 96.9(2) . . ?
O2 P1 C1 105.6(2) . . ?
O3 P1 C1 109.0(2) . . ?
O4 P2 O5 113.3(3) . . ?
O4 P2 O6 115.3(3) . . ?
O4 P2 C11 115.9(3) . . ?
O5 P2 C11 106.5(3) . . ?
O6 P2 O5 103.4(3) . . ?
O6 P2 C11 101.0(2) . . ?
C21 O2 P1 120.1(5) . . ?
C23 O3 P1 120.8(4) . . ?
C31 O5 P2 117.3(4) . . ?
C33 O6 P2 122.4(5) . . ?
C2 N1 Ni1 127.7(3) . . ?
C2 N1 C5 105.6(4) . . ?
C5 N1 Ni1 126.6(4) . . ?
C7 N2 Ni1 126.3(4) . . ?
C10 N2 Ni1 127.5(4) . . ?
C10 N2 C7 106.1(4) . . ?
C12 N3 Ni1 127.9(4) . . ?
C15 N3 Ni1 126.4(3) . . ?
C15 N3 C12 105.7(4) . . ?
C4 N4 Ni1 126.8(3) . . ?
C20 N4 Ni1 127.8(4) . . ?
C20 N4 C4 105.1(4) . . ?
C2 C1 P1 118.2(4) . . ?
C20 C1 P1 120.7(4) . . ?
C20 C1 C2 121.0(5) . . ?
N1 C2 C1 124.3(5) . . ?
N1 C2 C3 110.0(4) . . ?
C1 C2 C3 125.2(5) . . ?
C2 C3 H3 126.4 . . ?
C9 C3 C2 107.1(5) . . ?
C9 C3 H3 126.4 . . ?
N4 C4 C18 110.5(5) . . ?
C16 C4 N4 123.9(5) . . ?
C16 C4 C18 125.3(5) . . ?
N1 C5 C9 109.5(5) . . ?
C6 C5 N1 124.7(5) . . ?
C6 C5 C9 125.4(5) . . ?
C5 C6 C25A 111.9(5) . . ?
C5 C6 C25B 127.0(7) . . ?
C7 C6 C5 122.0(5) . . ?
C7 C6 C25A 125.4(5) . . ?
C7 C6 C25B 110.7(6) . . ?
N2 C7 C8 109.2(5) . . ?
C6 C7 N2 124.7(5) . . ?
C6 C7 C8 125.3(5) . . ?
C7 C8 H8 126.2 . . ?
C17 C8 C7 107.5(5) . . ?
C17 C8 H8 126.2 . . ?
C3 C9 C5 107.8(5) . . ?
C3 C9 H9 126.1 . . ?
C5 C9 H9 126.1 . . ?
N2 C10 C17 108.6(6) . . ?
C11 C10 N2 124.0(5) . . ?
C11 C10 C17 126.3(6) . . ?
C10 C11 P2 119.2(4) . . ?
C12 C11 P2 118.7(5) . . ?
C12 C11 C10 121.5(5) . . ?
N3 C12 C11 124.1(5) . . ?
N3 C12 C13 108.9(5) . . ?
C11 C12 C13 126.3(5) . . ?
C12 C13 H13 125.9 . . ?
C14 C13 C12 108.3(5) . . ?
C14 C13 H13 125.9 . . ?
C13 C14 H14 126.8 . . ?
C13 C14 C15 106.3(5) . . ?
C15 C14 H14 126.8 . . ?
N3 C15 C14 110.6(5) . . ?
N3 C15 C16 125.9(5) . . ?
C16 C15 C14 123.2(5) . . ?
C4 C16 C15 120.9(5) . . ?
C4 C16 C35 120.9(4) . . ?
C15 C16 C35 118.0(5) . . ?
C4 C18 H18 126.9 . . ?
C19 C18 C4 106.2(5) . . ?
C19 C18 H18 126.9 . . ?
C18 C19 H19 125.9 . . ?
C18 C19 C20 108.2(5) . . ?
C20 C19 H19 125.9 . . ?
N4 C20 C1 124.2(5) . . ?
N4 C20 C19 109.9(5) . . ?
C1 C20 C19 125.1(5) . . ?
O2 C21 H21A 109.6 . . ?
O2 C21 H21B 109.6 . . ?
H21A C21 H21B 108.2 . . ?
C22 C21 O2 110.1(8) . . ?
C22 C21 H21A 109.6 . . ?
C22 C21 H21B 109.6 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O3 C23 H23A 109.9 . . ?
O3 C23 H23B 109.9 . . ?
O3 C23 C24 109.1(6) . . ?
H23A C23 H23B 108.3 . . ?
C24 C23 H23A 109.9 . . ?
C24 C23 H23B 109.9 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26A C25A C6 120.6(5) . . ?
C26A C25A C30A 120.0 . . ?
C30A C25A C6 119.2(5) . . ?
C25A C26A H26A 120.0 . . ?
C25A C26A C27A 120.0 . . ?
C27A C26A H26A 120.0 . . ?
C26A C27A H27A 120.0 . . ?
C26A C27A C28A 120.0 . . ?
C28A C27A H27A 120.0 . . ?
C27A C28A H28A 120.0 . . ?
C29A C28A C27A 120.0 . . ?
C29A C28A H28A 120.0 . . ?
C28A C29A H29A 120.0 . . ?
C28A C29A C30A 120.0 . . ?
C30A C29A H29A 120.0 . . ?
C25A C30A H30A 120.0 . . ?
C29A C30A C25A 120.0 . . ?
C29A C30A H30A 120.0 . . ?
C26B C25B C6 122.3(8) . . ?
C26B C25B C30B 120.0 . . ?
C30B C25B C6 117.6(8) . . ?
C25B C26B H26B 120.0 . . ?
C27B C26B C25B 120.0 . . ?
C27B C26B H26B 120.0 . . ?
C26B C27B H27B 120.0 . . ?
C28B C27B C26B 120.0 . . ?
C28B C27B H27B 120.0 . . ?
C27B C28B H28B 120.0 . . ?
C27B C28B C29B 120.0 . . ?
C29B C28B H28B 120.0 . . ?
C28B C29B H29B 120.0 . . ?
C30B C29B C28B 120.0 . . ?
C30B C29B H29B 120.0 . . ?
C25B C30B H30B 120.0 . . ?
C29B C30B C25B 120.0 . . ?
C29B C30B H30B 120.0 . . ?
O5 C31 H31A 109.7 . . ?
O5 C31 H31B 109.7 . . ?
H31A C31 H31B 108.2 . . ?
C32 C31 O5 109.8(7) . . ?
C32 C31 H31A 109.7 . . ?
C32 C31 H31B 109.7 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O6 C33 H33A 110.2 . . ?
O6 C33 H33B 110.2 . . ?
O6 C33 C34 107.7(6) . . ?
H33A C33 H33B 108.5 . . ?
C34 C33 H33A 110.2 . . ?
C34 C33 H33B 110.2 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 C16 119.4(5) . . ?
C36 C35 C40 117.8(5) . . ?
C40 C35 C16 122.6(5) . . ?
C35 C36 H36 119.4 . . ?
C37 C36 C35 121.3(5) . . ?
C37 C36 H36 119.4 . . ?
C36 C37 H37 120.0 . . ?
C38 C37 C36 120.0(6) . . ?
C38 C37 H37 120.0 . . ?
C37 C38 H38 120.4 . . ?
C37 C38 C39 119.2(6) . . ?
C39 C38 H38 120.4 . . ?
C38 C39 H39 119.9 . . ?
C40 C39 C38 120.1(5) . . ?
C40 C39 H39 119.9 . . ?
C35 C40 H40 119.2 . . ?
C39 C40 C35 121.5(5) . . ?
C39 C40 H40 119.2 . . ?
C8 C17 C10 108.4(6) . . ?
C8 C17 H17 125.8 . . ?
C10 C17 H17 125.8 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C42 C41 H41A 109.5 . . ?
C42 C41 H41B 109.5 . . ?
C42 C41 H41C 109.5 . . ?
C41 C42 H42A 109.0 . . ?
C41 C42 H42B 109.0 . . ?
H42A C42 H42B 107.8 . . ?
C43 C42 C41 113.1(19) . . ?
C43 C42 H42A 109.0 . . ?
C43 C42 H42B 109.0 . . ?
C42 C43 C43 123(2) . 2_576 ?
C42 C43 H43A 106.5 . . ?
C42 C43 H43B 106.5 . . ?
C43 C43 H43A 106.5 2_576 . ?
C43 C43 H43B 106.5 2_576 . ?
H43A C43 H43B 106.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 N1 C2 C1 -12.1(8) . . . . ?
Ni1 N1 C2 C3 176.4(4) . . . . ?
Ni1 N1 C5 C6 -5.5(8) . . . . ?
Ni1 N1 C5 C9 -178.2(4) . . . . ?
Ni1 N2 C7 C6 15.0(8) . . . . ?
Ni1 N2 C7 C8 -174.9(4) . . . . ?
Ni1 N2 C10 C11 8.4(9) . . . . ?
Ni1 N2 C10 C17 176.7(4) . . . . ?
Ni1 N3 C12 C11 -11.3(8) . . . . ?
Ni1 N3 C12 C13 177.3(4) . . . . ?
Ni1 N3 C15 C14 -179.9(4) . . . . ?
Ni1 N3 C15 C16 -6.0(8) . . . . ?
Ni1 N4 C4 C16 14.3(7) . . . . ?
Ni1 N4 C4 C18 -171.9(3) . . . . ?
Ni1 N4 C20 C1 3.8(8) . . . . ?
Ni1 N4 C20 C19 173.9(4) . . . . ?
P1 O2 C21 C22 149.0(9) . . . . ?
P1 O3 C23 C24 159.2(5) . . . . ?
P1 C1 C2 N1 172.5(4) . . . . ?
P1 C1 C2 C3 -17.3(8) . . . . ?
P1 C1 C20 N4 -168.5(4) . . . . ?
P1 C1 C20 C19 22.8(8) . . . . ?
P2 O5 C31 C32 -170.2(6) . . . . ?
P2 O6 C33 C34 -169.1(6) . . . . ?
P2 C11 C12 N3 177.4(4) . . . . ?
P2 C11 C12 C13 -12.7(8) . . . . ?
O1 P1 O2 C21 54.7(6) . . . . ?
O1 P1 O3 C23 -58.0(5) . . . . ?
O1 P1 C1 C2 -171.7(5) . . . . ?
O1 P1 C1 C20 11.8(6) . . . . ?
O2 P1 O3 C23 179.2(5) . . . . ?
O2 P1 C1 C2 -44.6(5) . . . . ?
O2 P1 C1 C20 138.9(5) . . . . ?
O3 P1 O2 C21 177.5(5) . . . . ?
O3 P1 C1 C2 58.6(5) . . . . ?
O3 P1 C1 C20 -118.0(5) . . . . ?
O4 P2 O5 C31 -54.5(6) . . . . ?
O4 P2 O6 C33 -66.5(6) . . . . ?
O4 P2 C11 C10 15.8(6) . . . . ?
O4 P2 C11 C12 -172.8(4) . . . . ?
O5 P2 O6 C33 57.7(6) . . . . ?
O5 P2 C11 C10 -111.2(5) . . . . ?
O5 P2 C11 C12 60.2(5) . . . . ?
O6 P2 O5 C31 180.0(5) . . . . ?
O6 P2 C11 C10 141.1(5) . . . . ?
O6 P2 C11 C12 -47.5(5) . . . . ?
N1 C2 C3 C9 2.8(7) . . . . ?
N1 C5 C6 C7 -11.2(9) . . . . ?
N1 C5 C6 C25A 177.6(6) . . . . ?
N1 C5 C6 C25B 175.8(7) . . . . ?
N1 C5 C9 C3 2.2(7) . . . . ?
N2 Ni1 N3 C12 23.0(5) . . . . ?
N2 Ni1 N3 C15 -159.0(4) . . . . ?
N2 C7 C8 C17 -3.6(8) . . . . ?
N2 C10 C11 P2 -176.1(4) . . . . ?
N2 C10 C11 C12 12.7(9) . . . . ?
N2 C10 C17 C8 -1.3(8) . . . . ?
N3 C12 C13 C14 3.3(7) . . . . ?
N3 C15 C16 C4 -12.3(8) . . . . ?
N3 C15 C16 C35 173.5(5) . . . . ?
N4 Ni1 N3 C12 -158.3(5) . . . . ?
N4 Ni1 N3 C15 19.7(4) . . . . ?
N4 C4 C16 C15 7.9(8) . . . . ?
N4 C4 C16 C35 -178.0(5) . . . . ?
N4 C4 C18 C19 -3.7(6) . . . . ?
C1 P1 O2 C21 -70.5(6) . . . . ?
C1 P1 O3 C23 70.0(5) . . . . ?
C1 C2 C3 C9 -168.6(6) . . . . ?
C2 N1 C5 C6 172.4(5) . . . . ?
C2 N1 C5 C9 -0.4(6) . . . . ?
C2 C1 C20 N4 15.0(9) . . . . ?
C2 C1 C20 C19 -153.6(6) . . . . ?
C2 C3 C9 C5 -3.0(7) . . . . ?
C4 N4 C20 C1 -170.6(5) . . . . ?
C4 N4 C20 C19 -0.4(6) . . . . ?
C4 C16 C35 C36 126.2(6) . . . . ?
C4 C16 C35 C40 -58.0(7) . . . . ?
C4 C18 C19 C20 3.3(6) . . . . ?
C5 N1 C2 C1 170.0(6) . . . . ?
C5 N1 C2 C3 -1.4(6) . . . . ?
C5 C6 C7 N2 6.2(9) . . . . ?
C5 C6 C7 C8 -162.2(6) . . . . ?
C5 C6 C25A C26A -63.6(7) . . . . ?
C5 C6 C25A C30A 120.5(6) . . . . ?
C5 C6 C25B C26B -112.6(9) . . . . ?
C5 C6 C25B C30B 63.4(10) . . . . ?
C6 C5 C9 C3 -170.5(6) . . . . ?
C6 C7 C8 C17 166.3(6) . . . . ?
C6 C25A C26A C27A -175.9(7) . . . . ?
C6 C25A C30A C29A 175.9(7) . . . . ?
C6 C25B C26B C27B 175.8(10) . . . . ?
C6 C25B C30B C29B -176.0(10) . . . . ?
C7 N2 C10 C11 -169.3(6) . . . . ?
C7 N2 C10 C17 -1.0(7) . . . . ?
C7 C6 C25A C26A 125.6(6) . . . . ?
C7 C6 C25A C30A -50.3(8) . . . . ?
C7 C6 C25B C26B 73.7(9) . . . . ?
C7 C6 C25B C30B -110.3(8) . . . . ?
C7 C8 C17 C10 2.9(8) . . . . ?
C9 C5 C6 C7 160.5(6) . . . . ?
C9 C5 C6 C25A -10.7(8) . . . . ?
C9 C5 C6 C25B -12.5(11) . . . . ?
C10 N2 C7 C6 -167.3(6) . . . . ?
C10 N2 C7 C8 2.8(6) . . . . ?
C10 C11 C12 N3 -11.3(9) . . . . ?
C10 C11 C12 C13 158.5(6) . . . . ?
C11 P2 O5 C31 74.0(5) . . . . ?
C11 P2 O6 C33 167.8(6) . . . . ?
C11 C10 C17 C8 166.7(7) . . . . ?
C11 C12 C13 C14 -167.8(6) . . . . ?
C12 N3 C15 C14 -1.5(6) . . . . ?
C12 N3 C15 C16 172.4(5) . . . . ?
C12 C13 C14 C15 -4.1(7) . . . . ?
C13 C14 C15 N3 3.6(7) . . . . ?
C13 C14 C15 C16 -170.5(5) . . . . ?
C14 C15 C16 C4 160.8(5) . . . . ?
C14 C15 C16 C35 -13.4(8) . . . . ?
C15 N3 C12 C11 170.3(5) . . . . ?
C15 N3 C12 C13 -1.0(6) . . . . ?
C15 C16 C35 C36 -59.6(7) . . . . ?
C15 C16 C35 C40 116.2(6) . . . . ?
C16 C4 C18 C19 169.9(5) . . . . ?
C16 C35 C36 C37 176.4(6) . . . . ?
C16 C35 C40 C39 -177.1(5) . . . . ?
C18 C4 C16 C15 -164.9(5) . . . . ?
C18 C4 C16 C35 9.1(8) . . . . ?
C18 C19 C20 N4 -1.9(6) . . . . ?
C18 C19 C20 C1 168.2(5) . . . . ?
C20 N4 C4 C16 -171.2(5) . . . . ?
C20 N4 C4 C18 2.5(6) . . . . ?
C20 C1 C2 N1 -10.9(9) . . . . ?
C20 C1 C2 C3 159.3(6) . . . . ?
C25A C6 C7 N2 176.2(6) . . . . ?
C25A C6 C7 C8 7.8(10) . . . . ?
C25A C6 C25B C26B -119(3) . . . . ?
C25A C6 C25B C30B 57(2) . . . . ?
C25A C26A C27A C28A 0.0 . . . . ?
C26A C25A C30A C29A 0.0 . . . . ?
C26A C27A C28A C29A 0.0 . . . . ?
C27A C28A C29A C30A 0.0 . . . . ?
C28A C29A C30A C25A 0.0 . . . . ?
C30A C25A C26A C27A 0.0 . . . . ?
C25B C6 C7 N2 -179.7(7) . . . . ?
C25B C6 C7 C8 11.8(9) . . . . ?
C25B C6 C25A C26A 111(3) . . . . ?
C25B C6 C25A C30A -65(3) . . . . ?
C25B C26B C27B C28B 0.0 . . . . ?
C26B C25B C30B C29B 0.0 . . . . ?
C26B C27B C28B C29B 0.0 . . . . ?
C27B C28B C29B C30B 0.0 . . . . ?
C28B C29B C30B C25B 0.0 . . . . ?
C30B C25B C26B C27B 0.0 . . . . ?
C35 C36 C37 C38 0.0(10) . . . . ?
C36 C35 C40 C39 -1.2(9) . . . . ?
C36 C37 C38 C39 0.4(10) . . . . ?
C37 C38 C39 C40 -1.3(10) . . . . ?
C38 C39 C40 C35 1.7(10) . . . . ?
C40 C35 C36 C37 0.3(9) . . . . ?
C17 C10 C11 P2 17.7(9) . . . . ?
C17 C10 C11 C12 -153.5(7) . . . . ?
C41 C42 C43 C43 -174(2) . . . 2_576 ?

_database_code_depnum_ccdc_archive 'CCDC 998788'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_pd
_audit_creation_date             2014-04-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C40 H38 N4 O6 P2 Pd'
_chemical_formula_sum            'C40 H38 N4 O6 P2 Pd'
_chemical_formula_weight         839.08
_chemical_melting_point          ?
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_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'
'-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                   16.128(4)
_cell_length_b                   18.158(5)
_cell_length_c                   13.503(3)
_cell_angle_alpha                90
_cell_angle_beta                 113.570(3)
_cell_angle_gamma                90
_cell_volume                     3624.3(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2539
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.12
_cell_measurement_theta_min      2.76
_shelx_estimated_absorpt_T_max   0.937
_shelx_estimated_absorpt_T_min   0.914
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       ?
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.0982
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9482
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.998
_diffrn_reflns_theta_min         2.756
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3072
_reflns_number_total             4750
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.144
_refine_diff_density_min         -1.146
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         4750
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0442
_refine_ls_restrained_S_all      0.979
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0312P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0940
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14), C15(H15),
 C16(H16)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.2500 0.2500 0.5000 0.01664(9) Uani 1 2 d S T P . .
P1 P -0.08854(5) 0.20722(5) 0.45298(8) 0.0271(2) Uani 1 1 d . . . . .
O1 O -0.15093(15) 0.26907(13) 0.4146(2) 0.0409(7) Uani 1 1 d . . . . .
O2 O -0.11877(14) 0.13751(13) 0.37723(19) 0.0299(6) Uani 1 1 d . . . . .
O3 O -0.07809(14) 0.17578(14) 0.5653(2) 0.0326(6) Uani 1 1 d . . . . .
N1 N 0.13698(15) 0.31231(14) 0.4505(2) 0.0198(6) Uani 1 1 d . . . . .
N2 N 0.17995(16) 0.16681(14) 0.5295(2) 0.0194(6) Uani 1 1 d . . . . .
C1 C 0.12892(19) 0.38299(18) 0.4121(3) 0.0215(7) Uani 1 1 d . . . . .
C2 C 0.0384(2) 0.40860(19) 0.3839(3) 0.0300(8) Uani 1 1 d . . . . .
H2 H 0.0163 0.4550 0.3569 0.036 Uiso 1 1 calc R . . . .
C3 C -0.0087(2) 0.35435(19) 0.4034(3) 0.0295(8) Uani 1 1 d . . . . .
H3 H -0.0694 0.3558 0.3921 0.035 Uiso 1 1 calc R . . . .
C4 C 0.05201(19) 0.29306(18) 0.4450(3) 0.0212(7) Uani 1 1 d . . . . .
C5 C 0.02848(19) 0.22374(18) 0.4719(3) 0.0213(7) Uani 1 1 d . . . . .
C6 C 0.0891(2) 0.16472(18) 0.5092(3) 0.0215(7) Uani 1 1 d . . . . .
C7 C 0.0666(2) 0.09185(18) 0.5334(3) 0.0238(7) Uani 1 1 d . . . . .
H7 H 0.0096 0.0756 0.5254 0.029 Uiso 1 1 calc R . . . .
C8 C 0.1429(2) 0.05172(18) 0.5697(3) 0.0223(7) Uani 1 1 d . . . . .
H8 H 0.1485 0.0028 0.5918 0.027 Uiso 1 1 calc R . . . .
C9 C 0.2139(2) 0.09838(17) 0.5682(3) 0.0210(7) Uani 1 1 d . . . . .
C10 C 0.30345(19) 0.07549(17) 0.5991(3) 0.0204(7) Uani 1 1 d . . . . .
C11 C 0.32875(19) 0.00114(18) 0.6505(3) 0.0237(7) Uani 1 1 d . . . . .
C12 C 0.3347(2) -0.0090(2) 0.7551(3) 0.0316(8) Uani 1 1 d . . . . .
H12 H 0.3211 0.0295 0.7915 0.038 Uiso 1 1 calc R . . . .
C13 C 0.3609(3) -0.0765(2) 0.8049(4) 0.0456(11) Uani 1 1 d . . . . .
H13 H 0.3644 -0.0830 0.8748 0.055 Uiso 1 1 calc R . . . .
C14 C 0.3818(3) -0.1339(2) 0.7536(4) 0.0499(13) Uani 1 1 d . . . . .
H14 H 0.3998 -0.1789 0.7884 0.060 Uiso 1 1 calc R . . . .
C15 C 0.3758(3) -0.1244(2) 0.6490(4) 0.0461(11) Uani 1 1 d . . . . .
H15 H 0.3890 -0.1634 0.6130 0.055 Uiso 1 1 calc R . . . .
C16 C 0.3502(2) -0.0569(2) 0.5983(3) 0.0362(9) Uani 1 1 d . . . . .
H16 H 0.3474 -0.0505 0.5287 0.043 Uiso 1 1 calc R . . . .
C17 C -0.1330(3) 0.1459(2) 0.2640(3) 0.0444(11) Uani 1 1 d . . . . .
H17A H -0.0882 0.1792 0.2579 0.053 Uiso 1 1 calc R . . . .
H17B H -0.1926 0.1662 0.2229 0.053 Uiso 1 1 calc R . . . .
C18 C -0.1247(3) 0.0720(2) 0.2211(3) 0.0490(11) Uani 1 1 d . . . . .
H18A H -0.1306 0.0767 0.1477 0.074 Uiso 1 1 calc GR . . . .
H18B H -0.1714 0.0402 0.2235 0.074 Uiso 1 1 calc GR . . . .
H18C H -0.0666 0.0513 0.2643 0.074 Uiso 1 1 calc GR . . . .
C19 C -0.1586(2) 0.1641(3) 0.5863(4) 0.0501(12) Uani 1 1 d . . . . .
H19A H -0.1936 0.2092 0.5720 0.060 Uiso 1 1 calc R . . . .
H19B H -0.1957 0.1263 0.5382 0.060 Uiso 1 1 calc R . . . .
C20 C -0.1351(3) 0.1421(3) 0.6962(4) 0.0787(19) Uani 1 1 d . . . . .
H20A H -0.1892 0.1358 0.7087 0.118 Uiso 1 1 calc GR . . . .
H20B H -0.0981 0.1794 0.7438 0.118 Uiso 1 1 calc GR . . . .
H20C H -0.1023 0.0965 0.7096 0.118 Uiso 1 1 calc GR . . . .


_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 N1 2.019(2) . ?
Pd1 N1 2.019(2) 7_556 ?
Pd1 N2 2.019(2) . ?
Pd1 N2 2.019(2) 7_556 ?
P1 O1 1.458(3) . ?
P1 O2 1.577(3) . ?
P1 O3 1.565(3) . ?
P1 C5 1.825(3) . ?
O2 C17 1.461(4) . ?
O3 C19 1.451(4) . ?
N1 C1 1.371(4) . ?
N1 C4 1.387(4) . ?
N2 C6 1.379(4) . ?
N2 C9 1.374(4) . ?
C1 C2 1.431(4) . ?
C1 C10 1.383(4) 7_556 ?
C2 C3 1.332(5) . ?
C3 C4 1.440(4) . ?
C4 C5 1.404(5) . ?
C5 C6 1.402(4) . ?
C6 C7 1.444(4) . ?
C7 C8 1.342(4) . ?
C8 C9 1.432(4) . ?
C9 C10 1.396(4) . ?
C10 C1 1.383(4) 7_556 ?
C10 C11 1.498(4) . ?
C11 C12 1.390(5) . ?
C11 C16 1.387(5) . ?
C12 C13 1.379(5) . ?
C13 C14 1.367(6) . ?
C14 C15 1.387(6) . ?
C15 C16 1.383(5) . ?
C17 C18 1.489(6) . ?
C19 C20 1.433(6) . ?

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 Pd1 N1 180.0 . 7_556 ?
N1 Pd1 N2 91.01(10) . 7_556 ?
N1 Pd1 N2 88.99(10) 7_556 7_556 ?
N1 Pd1 N2 91.01(10) 7_556 . ?
N1 Pd1 N2 88.99(10) . . ?
N2 Pd1 N2 180.0 . 7_556 ?
O1 P1 O2 113.41(15) . . ?
O1 P1 O3 114.64(15) . . ?
O1 P1 C5 116.82(14) . . ?
O2 P1 C5 104.89(14) . . ?
O3 P1 O2 102.79(14) . . ?
O3 P1 C5 102.69(14) . . ?
C17 O2 P1 118.3(2) . . ?
C19 O3 P1 119.0(2) . . ?
C1 N1 Pd1 125.9(2) . . ?
C1 N1 C4 105.9(2) . . ?
C4 N1 Pd1 128.2(2) . . ?
C6 N2 Pd1 128.0(2) . . ?
C9 N2 Pd1 125.57(19) . . ?
C9 N2 C6 106.4(2) . . ?
N1 C1 C2 109.7(3) . . ?
N1 C1 C10 126.3(3) . 7_556 ?
C10 C1 C2 124.0(3) 7_556 . ?
C3 C2 C1 108.0(3) . . ?
C2 C3 C4 107.2(3) . . ?
N1 C4 C3 109.2(3) . . ?
N1 C4 C5 125.2(3) . . ?
C5 C4 C3 125.6(3) . . ?
C4 C5 P1 118.9(2) . . ?
C6 C5 P1 117.3(2) . . ?
C6 C5 C4 123.8(3) . . ?
N2 C6 C5 125.7(3) . . ?
N2 C6 C7 108.9(3) . . ?
C5 C6 C7 125.4(3) . . ?
C8 C7 C6 107.7(3) . . ?
C7 C8 C9 107.2(3) . . ?
N2 C9 C8 109.9(3) . . ?
N2 C9 C10 126.2(3) . . ?
C10 C9 C8 123.9(3) . . ?
C1 C10 C9 124.8(3) 7_556 . ?
C1 C10 C11 117.5(3) 7_556 . ?
C9 C10 C11 117.7(3) . . ?
C12 C11 C10 119.1(3) . . ?
C16 C11 C10 121.8(3) . . ?
C16 C11 C12 119.0(3) . . ?
C13 C12 C11 119.8(4) . . ?
C14 C13 C12 121.3(4) . . ?
C13 C14 C15 119.4(4) . . ?
C16 C15 C14 119.9(4) . . ?
C15 C16 C11 120.5(4) . . ?
O2 C17 C18 108.2(3) . . ?
C20 C19 O3 110.9(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 N1 C1 C2 179.4(2) . . . . ?
Pd1 N1 C1 C10 -0.4(5) . . . 7_556 ?
Pd1 N1 C4 C3 -179.1(2) . . . . ?
Pd1 N1 C4 C5 -1.5(5) . . . . ?
Pd1 N2 C6 C5 -6.0(5) . . . . ?
Pd1 N2 C6 C7 174.5(2) . . . . ?
Pd1 N2 C9 C8 -174.8(2) . . . . ?
Pd1 N2 C9 C10 3.5(5) . . . . ?
P1 O2 C17 C18 157.9(2) . . . . ?
P1 O3 C19 C20 -174.3(4) . . . . ?
P1 C5 C6 N2 -179.2(3) . . . . ?
P1 C5 C6 C7 0.3(5) . . . . ?
O1 P1 O2 C17 57.2(3) . . . . ?
O1 P1 O3 C19 44.8(3) . . . . ?
O1 P1 C5 C4 -2.5(3) . . . . ?
O1 P1 C5 C6 179.8(3) . . . . ?
O2 P1 O3 C19 -78.7(3) . . . . ?
O2 P1 C5 C4 124.0(3) . . . . ?
O2 P1 C5 C6 -53.7(3) . . . . ?
O3 P1 O2 C17 -178.5(2) . . . . ?
O3 P1 C5 C4 -128.9(3) . . . . ?
O3 P1 C5 C6 53.4(3) . . . . ?
N1 C1 C2 C3 -0.8(4) . . . . ?
N1 C4 C5 P1 -176.9(3) . . . . ?
N1 C4 C5 C6 0.7(5) . . . . ?
N2 C6 C7 C8 1.3(4) . . . . ?
N2 C9 C10 C1 -5.1(6) . . . 7_556 ?
N2 C9 C10 C11 173.5(3) . . . . ?
C1 N1 C4 C3 -0.7(4) . . . . ?
C1 N1 C4 C5 177.0(3) . . . . ?
C1 C2 C3 C4 0.3(4) . . . . ?
C1 C10 C11 C12 106.6(4) 7_556 . . . ?
C1 C10 C11 C16 -70.5(4) 7_556 . . . ?
C2 C3 C4 N1 0.3(4) . . . . ?
C2 C3 C4 C5 -177.4(4) . . . . ?
C3 C4 C5 P1 0.4(5) . . . . ?
C3 C4 C5 C6 178.0(3) . . . . ?
C4 N1 C1 C2 0.9(4) . . . . ?
C4 N1 C1 C10 -178.9(3) . . . 7_556 ?
C4 C5 C6 N2 3.2(5) . . . . ?
C4 C5 C6 C7 -177.3(3) . . . . ?
C5 P1 O2 C17 -71.4(3) . . . . ?
C5 P1 O3 C19 172.5(3) . . . . ?
C5 C6 C7 C8 -178.2(3) . . . . ?
C6 N2 C9 C8 1.5(4) . . . . ?
C6 N2 C9 C10 179.8(3) . . . . ?
C6 C7 C8 C9 -0.4(4) . . . . ?
C7 C8 C9 N2 -0.7(4) . . . . ?
C7 C8 C9 C10 -179.1(3) . . . . ?
C8 C9 C10 C1 173.1(3) . . . 7_556 ?
C8 C9 C10 C11 -8.4(5) . . . . ?
C9 N2 C6 C5 177.8(3) . . . . ?
C9 N2 C6 C7 -1.7(4) . . . . ?
C9 C10 C11 C12 -72.0(4) . . . . ?
C9 C10 C11 C16 110.9(4) . . . . ?
C10 C1 C2 C3 179.0(3) 7_556 . . . ?
C10 C11 C12 C13 -177.8(3) . . . . ?
C10 C11 C16 C15 178.2(3) . . . . ?
C11 C12 C13 C14 0.4(5) . . . . ?
C12 C11 C16 C15 1.0(5) . . . . ?
C12 C13 C14 C15 -0.5(6) . . . . ?
C13 C14 C15 C16 1.0(6) . . . . ?
C14 C15 C16 C11 -1.2(6) . . . . ?
C16 C11 C12 C13 -0.6(5) . . . . ?

_database_code_depnum_ccdc_archive 'CCDC 998789'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_cd
_audit_creation_date             2014-04-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.5(C80 H76 Cd2 N8 O12 P4)'
_chemical_formula_sum            'C40 H38 Cd N4 O6 P2'
_chemical_formula_weight         845.08
_chemical_melting_point          ?
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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.4567(16)
_cell_length_b                   11.7829(15)
_cell_length_c                   12.1147(16)
_cell_angle_alpha                90
_cell_angle_beta                 91.889(2)
_cell_angle_gamma                90
_cell_volume                     1777.2(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   0.914
_shelx_estimated_absorpt_T_min   0.888
_exptl_absorpt_coefficient_mu    0.760
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       ?
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18896
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.997
_diffrn_reflns_theta_min         2.380
_diffrn_ambient_temperature      153.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3675
_reflns_number_total             4664
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_refine_diff_density_max         1.273
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         4664
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0333
_refine_ls_restrained_S_all      0.967
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0431P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0827
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C11(H11), C12(H12), C16(H16), C17(H17), C18(H18), C19(H19),
 C20(H20)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.5000 1.0000 0.5000 0.03079(8) Uani 1 2 d S T P . .
P1 P 0.36450(4) 1.23660(5) 0.15006(4) 0.02329(12) Uani 1 1 d . . . . .
N1 N 0.35915(13) 1.00172(12) 0.39398(13) 0.0169(3) Uani 1 1 d . . . . .
N2 N 0.57004(12) 1.12530(13) 0.39508(13) 0.0183(3) Uani 1 1 d . . . . .
O1 O 0.44135(12) 1.31440(13) 0.10163(13) 0.0311(4) Uani 1 1 d . . . . .
O2 O 0.31934(12) 1.14617(14) 0.06443(12) 0.0331(4) Uani 1 1 d . . . . .
O3 O 0.25834(12) 1.29542(13) 0.18666(12) 0.0300(3) Uani 1 1 d . . . . .
C1 C 0.27125(14) 0.93545(15) 0.40956(15) 0.0171(4) Uani 1 1 d . . . . .
C2 C 0.18811(16) 0.96956(17) 0.33018(16) 0.0211(4) Uani 1 1 d . . . . .
H2 H 0.1181 0.9379 0.3222 0.025 Uiso 1 1 calc R . . . .
C3 C 0.22851(16) 1.05502(17) 0.26927(17) 0.0231(4) Uani 1 1 d . . . . .
H3 H 0.1920 1.0946 0.2109 0.028 Uiso 1 1 calc R . . . .
C4 C 0.33825(14) 1.07501(15) 0.30976(15) 0.0171(4) Uani 1 1 d . . . . .
C5 C 0.41154(15) 1.15801(15) 0.27029(16) 0.0192(4) Uani 1 1 d . . . . .
C6 C 0.3902(3) 1.0847(3) 0.0017(3) 0.0675(10) Uani 1 1 d . . . . .
H6A H 0.4308 1.0307 0.0497 0.081 Uiso 1 1 calc R . . . .
H6B H 0.4423 1.1370 -0.0316 0.081 Uiso 1 1 calc R . . . .
C7 C 0.3296(3) 1.0203(3) -0.0885(3) 0.0609(9) Uani 1 1 d . . . . .
H7A H 0.3789 0.9687 -0.1251 0.091 Uiso 1 1 calc GR . . . .
H7B H 0.2991 1.0741 -0.1427 0.091 Uiso 1 1 calc GR . . . .
H7C H 0.2717 0.9765 -0.0563 0.091 Uiso 1 1 calc GR . . . .
C8 C 0.21325(19) 1.3830(2) 0.1134(2) 0.0378(6) Uani 1 1 d . . . . .
H8A H 0.2050 1.3532 0.0372 0.045 Uiso 1 1 calc R . . . .
H8B H 0.2619 1.4494 0.1125 0.045 Uiso 1 1 calc R . . . .
C9 C 0.1079(2) 1.4168(2) 0.1541(2) 0.0424(6) Uani 1 1 d . . . . .
H9A H 0.0763 1.4751 0.1054 0.064 Uiso 1 1 calc GR . . . .
H9B H 0.1170 1.4473 0.2292 0.064 Uiso 1 1 calc GR . . . .
H9C H 0.0604 1.3506 0.1550 0.064 Uiso 1 1 calc GR . . . .
C10 C 0.51594(15) 1.18527(16) 0.31497(16) 0.0187(4) Uani 1 1 d . . . . .
C11 C 0.58010(16) 1.28485(17) 0.28920(17) 0.0260(4) Uani 1 1 d . . . . .
H11 H 0.5628 1.3410 0.2352 0.031 Uiso 1 1 calc R . . . .
C12 C 0.66840(17) 1.28229(17) 0.35616(17) 0.0251(4) Uani 1 1 d . . . . .
H12 H 0.7247 1.3367 0.3583 0.030 Uiso 1 1 calc R . . . .
C13 C 0.66230(15) 1.18163(15) 0.42434(15) 0.0182(4) Uani 1 1 d . . . . .
C14 C 0.73728(15) 1.15127(15) 0.50984(16) 0.0181(4) Uani 1 1 d . . . . .
C15 C 0.83852(15) 1.22070(16) 0.51575(16) 0.0205(4) Uani 1 1 d . . . . .
C16 C 0.90775(17) 1.22149(19) 0.42798(18) 0.0279(5) Uani 1 1 d . . . . .
H16 H 0.8908 1.1771 0.3643 0.033 Uiso 1 1 calc R . . . .
C17 C 1.00057(18) 1.2854(2) 0.4315(2) 0.0355(5) Uani 1 1 d . . . . .
H17 H 1.0476 1.2836 0.3714 0.043 Uiso 1 1 calc R . . . .
C18 C 1.02506(19) 1.3525(2) 0.5230(2) 0.0363(6) Uani 1 1 d . . . . .
H18 H 1.0880 1.3980 0.5253 0.044 Uiso 1 1 calc R . . . .
C19 C 0.95734(18) 1.35251(18) 0.6108(2) 0.0322(5) Uani 1 1 d . . . . .
H19 H 0.9743 1.3977 0.6739 0.039 Uiso 1 1 calc R . . . .
C20 C 0.86443(16) 1.28709(17) 0.60774(18) 0.0251(4) Uani 1 1 d . . . . .
H20 H 0.8184 1.2877 0.6687 0.030 Uiso 1 1 calc R . . . .


_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
Cd1 N1 2.1401(16) . ?
Cd1 N1 2.1401(16) 3_676 ?
Cd1 N2 2.1516(15) 3_676 ?
Cd1 N2 2.1516(15) . ?
Cd1 O1 2.6252(14) 4_586 ?
Cd1 O1 2.6252(14) 2_645 ?
P1 O1 1.4622(15) . ?
P1 O2 1.5779(16) . ?
P1 O3 1.5698(16) . ?
P1 C5 1.8073(19) . ?
N1 C1 1.363(2) . ?
N1 C4 1.355(2) . ?
N2 C10 1.361(2) . ?
N2 C13 1.364(2) . ?
O1 Cd1 2.6252(14) 2_655 ?
O2 C6 1.388(3) . ?
O3 C8 1.461(3) . ?
C1 C2 1.447(3) . ?
C1 C14 1.420(3) 3_676 ?
C2 C3 1.355(3) . ?
C3 C4 1.456(3) . ?
C4 C5 1.431(3) . ?
C5 C10 1.429(3) . ?
C6 C7 1.512(4) . ?
C8 C9 1.472(3) . ?
C10 C11 1.459(3) . ?
C11 C12 1.345(3) . ?
C12 C13 1.449(3) . ?
C13 C14 1.418(3) . ?
C14 C1 1.420(3) 3_676 ?
C14 C15 1.503(3) . ?
C15 C16 1.391(3) . ?
C15 C20 1.391(3) . ?
C16 C17 1.380(3) . ?
C17 C18 1.387(4) . ?
C18 C19 1.379(3) . ?
C19 C20 1.390(3) . ?

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 Cd1 N1 180.0 . 3_676 ?
N1 Cd1 N2 88.82(6) 3_676 3_676 ?
N1 Cd1 N2 91.18(6) 3_676 . ?
N1 Cd1 N2 91.19(6) . 3_676 ?
N1 Cd1 N2 88.82(6) . . ?
N1 Cd1 O1 92.19(5) . 4_586 ?
N1 Cd1 O1 92.19(5) 3_676 2_645 ?
N1 Cd1 O1 87.81(5) . 2_645 ?
N1 Cd1 O1 87.81(5) 3_676 4_586 ?
N2 Cd1 N2 180.0 3_676 . ?
N2 Cd1 O1 99.79(6) . 2_645 ?
N2 Cd1 O1 80.21(6) . 4_586 ?
N2 Cd1 O1 99.79(5) 3_676 4_586 ?
N2 Cd1 O1 80.21(5) 3_676 2_645 ?
O1 Cd1 O1 180.00(6) 4_586 2_645 ?
O1 P1 O2 112.55(9) . . ?
O1 P1 O3 113.91(9) . . ?
O1 P1 C5 116.45(9) . . ?
O2 P1 C5 106.43(9) . . ?
O3 P1 O2 101.44(9) . . ?
O3 P1 C5 104.62(8) . . ?
C1 N1 Cd1 123.91(12) . . ?
C4 N1 Cd1 126.24(12) . . ?
C4 N1 C1 109.51(15) . . ?
C10 N2 Cd1 125.22(12) . . ?
C10 N2 C13 109.01(15) . . ?
C13 N2 Cd1 122.35(12) . . ?
P1 O1 Cd1 155.02(9) . 2_655 ?
C6 O2 P1 119.53(17) . . ?
C8 O3 P1 116.80(14) . . ?
N1 C1 C2 108.03(16) . . ?
N1 C1 C14 125.89(17) . 3_676 ?
C14 C1 C2 126.08(17) 3_676 . ?
C3 C2 C1 107.33(17) . . ?
C2 C3 C4 107.35(17) . . ?
N1 C4 C3 107.78(16) . . ?
N1 C4 C5 125.32(16) . . ?
C5 C4 C3 126.89(17) . . ?
C4 C5 P1 115.22(14) . . ?
C10 C5 P1 117.19(14) . . ?
C10 C5 C4 127.59(17) . . ?
O2 C6 C7 110.2(3) . . ?
O3 C8 C9 108.47(19) . . ?
N2 C10 C5 125.21(17) . . ?
N2 C10 C11 107.96(16) . . ?
C5 C10 C11 126.72(18) . . ?
C12 C11 C10 107.19(17) . . ?
C11 C12 C13 107.75(18) . . ?
N2 C13 C12 108.05(16) . . ?
N2 C13 C14 126.60(16) . . ?
C14 C13 C12 125.28(17) . . ?
C1 C14 C15 116.15(16) 3_676 . ?
C13 C14 C1 128.45(17) . 3_676 ?
C13 C14 C15 115.40(16) . . ?
C16 C15 C14 120.51(18) . . ?
C20 C15 C14 121.10(18) . . ?
C20 C15 C16 118.38(18) . . ?
C17 C16 C15 121.3(2) . . ?
C16 C17 C18 119.9(2) . . ?
C19 C18 C17 119.5(2) . . ?
C18 C19 C20 120.6(2) . . ?
C19 C20 C15 120.3(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cd1 N1 C1 C2 173.21(12) . . . . ?
Cd1 N1 C1 C14 -6.4(3) . . . 3_676 ?
Cd1 N1 C4 C3 -172.84(12) . . . . ?
Cd1 N1 C4 C5 6.1(3) . . . . ?
Cd1 N2 C10 C5 -15.0(3) . . . . ?
Cd1 N2 C10 C11 161.25(13) . . . . ?
Cd1 N2 C13 C12 -161.71(13) . . . . ?
Cd1 N2 C13 C14 15.5(3) . . . . ?
P1 O2 C6 C7 -169.4(2) . . . . ?
P1 O3 C8 C9 172.79(17) . . . . ?
P1 C5 C10 N2 -170.63(15) . . . . ?
P1 C5 C10 C11 13.8(3) . . . . ?
N1 C1 C2 C3 0.1(2) . . . . ?
N1 C4 C5 P1 175.60(14) . . . . ?
N1 C4 C5 C10 -4.6(3) . . . . ?
N2 C10 C11 C12 -1.4(2) . . . . ?
N2 C13 C14 C1 -7.2(3) . . . 3_676 ?
N2 C13 C14 C15 173.18(18) . . . . ?
O1 P1 O2 C6 49.8(2) . . . . ?
O1 P1 O3 C8 39.95(18) . . . . ?
O1 P1 C5 C4 -174.45(14) . . . . ?
O1 P1 C5 C10 5.71(19) . . . . ?
O2 P1 O1 Cd1 90.8(2) . . . 2_655 ?
O2 P1 O3 C8 -81.23(17) . . . . ?
O2 P1 C5 C4 -48.05(16) . . . . ?
O2 P1 C5 C10 132.11(15) . . . . ?
O3 P1 O1 Cd1 -24.0(3) . . . 2_655 ?
O3 P1 O2 C6 171.9(2) . . . . ?
O3 P1 C5 C4 58.84(16) . . . . ?
O3 P1 C5 C10 -120.99(15) . . . . ?
C1 N1 C4 C3 0.7(2) . . . . ?
C1 N1 C4 C5 179.64(17) . . . . ?
C1 C2 C3 C4 0.3(2) . . . . ?
C1 C14 C15 C16 118.5(2) 3_676 . . . ?
C1 C14 C15 C20 -62.6(2) 3_676 . . . ?
C2 C3 C4 N1 -0.6(2) . . . . ?
C2 C3 C4 C5 -179.55(19) . . . . ?
C3 C4 C5 P1 -5.6(3) . . . . ?
C3 C4 C5 C10 174.2(2) . . . . ?
C4 N1 C1 C2 -0.5(2) . . . . ?
C4 N1 C1 C14 179.92(17) . . . 3_676 ?
C4 C5 C10 N2 9.6(3) . . . . ?
C4 C5 C10 C11 -166.0(2) . . . . ?
C5 P1 O1 Cd1 -145.9(2) . . . 2_655 ?
C5 P1 O2 C6 -78.9(2) . . . . ?
C5 P1 O3 C8 168.21(16) . . . . ?
C5 C10 C11 C12 174.8(2) . . . . ?
C10 N2 C13 C12 -1.6(2) . . . . ?
C10 N2 C13 C14 175.54(18) . . . . ?
C10 C11 C12 C13 0.4(2) . . . . ?
C11 C12 C13 N2 0.7(2) . . . . ?
C11 C12 C13 C14 -176.49(19) . . . . ?
C12 C13 C14 C1 169.54(19) . . . 3_676 ?
C12 C13 C14 C15 -10.1(3) . . . . ?
C13 N2 C10 C5 -174.39(18) . . . . ?
C13 N2 C10 C11 1.9(2) . . . . ?
C13 C14 C15 C16 -61.8(2) . . . . ?
C13 C14 C15 C20 117.1(2) . . . . ?
C14 C1 C2 C3 179.69(19) 3_676 . . . ?
C14 C15 C16 C17 179.4(2) . . . . ?
C14 C15 C20 C19 -178.70(18) . . . . ?
C15 C16 C17 C18 -1.4(4) . . . . ?
C16 C15 C20 C19 0.2(3) . . . . ?
C16 C17 C18 C19 1.4(4) . . . . ?
C17 C18 C19 C20 -0.7(4) . . . . ?
C18 C19 C20 C15 -0.1(3) . . . . ?
C20 C15 C16 C17 0.6(3) . . . . ?

_database_code_depnum_ccdc_archive 'CCDC 998790'
