#------------------------------------------------------------------------------
#$Date: 2015-07-11 00:45:06 +0300 (Sat, 11 Jul 2015) $
#$Revision: 143592 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/48/7034854.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7034854
loop_
_publ_author_name
'Jevtovikj, Ivana'
'Manzini, Simone'
'Hanauer, Matthias'
'Rominger, Frank'
'Schaub, Thomas'
_publ_section_title
;
 Investigations on the catalytic carboxylation of olefins with CO2 towards
 α,β-unsaturated carboxylic acid salts: characterization of
 intermediates and ligands as well as substrate effects.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11083
_journal_page_last               11094
_journal_paper_doi               10.1039/c5dt01040c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C31 H54 Ni O2 P2'
_chemical_formula_weight         579.39
_chemical_name_common            '4c in manuscript'
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-03-05 deposited with the CCDC.
2015-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.6368(16)
_cell_length_b                   21.6435(12)
_cell_length_c                   9.1291(4)
_cell_measurement_reflns_used    5292
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      21.34
_cell_measurement_theta_min      2.28
_cell_volume                     6251.0(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.770
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II Quazar area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0843
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_laue_measured_fraction_full 0.770
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            40500
_diffrn_reflns_point_group_measured_fraction_full 0.770
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         22.984
_diffrn_reflns_theta_min         1.287
_diffrn_source                   'ImuS microsource'
_exptl_absorpt_coefficient_mu    0.748
_exptl_absorpt_correction_T_max  0.9412
_exptl_absorpt_correction_T_min  0.8798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2008). SADABS. University of Göttingen, Germany.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         4469
_refine_ls_number_restraints     528
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1209
_refine_ls_R_factor_gt           0.0765
_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)+(0.0630P)²+20.3407P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1733
_refine_ls_wR_factor_ref         0.1969
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2880
_reflns_number_total             4469
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt01040c2.cif
_cod_data_source_block           ij21
_cod_depositor_comments
'Adding full bibliography for 7034853--7034856.cif.'
_cod_database_code               7034854
_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. 
;
_shelx_estimated_absorpt_t_min   0.909
_shelx_estimated_absorpt_t_max   0.929
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
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_1 Ni 0.33877(3) 0.7500 1.01220(11) 0.0573(4) Uani 1 2 d DS TU P A .
P1_1 P 0.30469(5) 0.68027(9) 0.8932(2) 0.0648(6) Uani 1 1 d D U . . .
C1_1 C 0.3869(4) 0.6804(7) 1.0629(16) 0.056(4) Uani 0.5 1 d D U P A -1
H1A_1 H 0.3885 0.6655 1.1652 0.067 Uiso 0.5 1 calc R U P A -1
H1B_1 H 0.3926 0.6484 0.9878 0.067 Uiso 0.5 1 calc R U P A -1
C2_1 C 0.4015(3) 0.7416(13) 1.0338(11) 0.050(4) Uani 0.5 1 d D U P A -1
H2_1 H 0.4205 0.7497 0.9484 0.060 Uiso 0.5 1 calc R U P A -1
C3_1 C 0.3872(4) 0.7896(7) 1.1176(14) 0.053(3) Uani 0.5 1 d D U P A -1
H3_1 H 0.3951 0.8317 1.0821 0.063 Uiso 0.5 1 calc R U P A -1
C4_1 C 0.3764(4) 0.7854(6) 1.2781(12) 0.065(3) Uani 0.5 1 d D U P A -1
H4A_1 H 0.3806 0.8268 1.3219 0.079 Uiso 0.5 1 calc R U P A -1
H4B_1 H 0.3970 0.7572 1.3250 0.079 Uiso 0.5 1 calc R U P A -1
C5_1 C 0.3323(4) 0.7635(8) 1.3178(11) 0.061(4) Uani 0.5 1 d D U P A -1
O5_1 O 0.3137(2) 0.7318(4) 1.2226(8) 0.060(3) Uani 0.5 1 d D U P A -1
O6_1 O 0.3183(3) 0.7774(5) 1.4384(9) 0.093(4) Uani 0.5 1 d D U P A -1
C10_1 C 0.2612(5) 0.7261(7) 0.7883(19) 0.054(4) Uani 0.5 1 d D U P B -1
H10A_1 H 0.2537 0.7033 0.6979 0.065 Uiso 0.5 1 calc R U P B -1
H10B_1 H 0.2355 0.7284 0.8501 0.065 Uiso 0.5 1 calc R U P B -1
C9_1 C 0.2744(5) 0.7899(8) 0.748(2) 0.060(5) Uani 0.5 1 d D U P . .
H9A_1 H 0.2492 0.8161 0.7316 0.072 Uiso 0.5 1 calc R U P B .
H9B_1 H 0.2913 0.7891 0.6571 0.072 Uiso 0.5 1 calc R U P . .
C11_1 C 0.2709(2) 0.6272(3) 1.0018(9) 0.082(2) Uani 1 1 d D U . . .
H11_1 H 0.2560 0.5987 0.9328 0.098 Uiso 1 1 calc R U . . .
C12_1 C 0.2984(2) 0.5888(4) 1.1040(9) 0.088(3) Uani 1 1 d D U . . .
H12A_1 H 0.3142 0.6166 1.1704 0.105 Uiso 1 1 calc R U . . .
H12B_1 H 0.3192 0.5651 1.0455 0.105 Uiso 1 1 calc R U . . .
C13_1 C 0.2715(3) 0.5436(4) 1.1958(12) 0.123(4) Uani 1 1 d D U . . .
H13A_1 H 0.2571 0.5137 1.1304 0.148 Uiso 1 1 calc R U . . .
H13B_1 H 0.2899 0.5201 1.2634 0.148 Uiso 1 1 calc R U . . .
C14_1 C 0.2388(3) 0.5796(4) 1.2829(12) 0.135(4) Uani 1 1 d D U . . .
H14A_1 H 0.2210 0.5506 1.3393 0.162 Uiso 1 1 calc R U . . .
H14B_1 H 0.2534 0.6072 1.3533 0.162 Uiso 1 1 calc R U . . .
C15_1 C 0.2111(2) 0.6180(4) 1.1823(12) 0.124(4) Uani 1 1 d D U . . .
H15A_1 H 0.1906 0.6419 1.2415 0.149 Uiso 1 1 calc R U . . .
H15B_1 H 0.1950 0.5903 1.1166 0.149 Uiso 1 1 calc R U . . .
C16_1 C 0.2379(2) 0.6623(3) 1.0904(11) 0.100(3) Uani 1 1 d D U . . .
H16A_1 H 0.2194 0.6858 1.0232 0.120 Uiso 1 1 calc R U . . .
H16B_1 H 0.2522 0.6922 1.1558 0.120 Uiso 1 1 calc R U . . .
C21_1 C 0.3365(2) 0.6280(4) 0.7753(10) 0.094(3) Uani 1 1 d D U . . .
H21_1 H 0.3524 0.6005 0.8438 0.112 Uiso 1 1 calc R U . . .
C22_1 C 0.3100(3) 0.5852(5) 0.6796(13) 0.135(4) Uani 1 1 d D U . . .
H22A_1 H 0.2923 0.6101 0.6124 0.163 Uiso 1 1 calc R U . . .
H22B_1 H 0.2910 0.5602 0.7422 0.163 Uiso 1 1 calc R U . . .
C23_1 C 0.3390(4) 0.5415(6) 0.5887(17) 0.193(6) Uani 1 1 d D U . . .
H23A_1 H 0.3528 0.5118 0.6559 0.232 Uiso 1 1 calc R U . . .
H23B_1 H 0.3213 0.5176 0.5195 0.232 Uiso 1 1 calc R U . . .
C24_1 C 0.3712(4) 0.5736(6) 0.5073(15) 0.197(6) Uani 1 1 d D U . . .
H24A_1 H 0.3577 0.5972 0.4271 0.236 Uiso 1 1 calc R U . . .
H24B_1 H 0.3905 0.5430 0.4624 0.236 Uiso 1 1 calc R U . . .
C25_1 C 0.3970(3) 0.6179(5) 0.6019(13) 0.149(5) Uani 1 1 d D U . . .
H25A_1 H 0.4147 0.5938 0.6709 0.179 Uiso 1 1 calc R U . . .
H25B_1 H 0.4162 0.6422 0.5383 0.179 Uiso 1 1 calc R U . . .
C26_1 C 0.3694(3) 0.6615(4) 0.6874(10) 0.113(3) Uani 1 1 d D U . . .
H26A_1 H 0.3872 0.6864 0.7542 0.135 Uiso 1 1 calc R U . . .
H26B_1 H 0.3552 0.6902 0.6187 0.135 Uiso 1 1 calc R U . . .
Ni1_2 Ni 0.45924(3) 0.2500 0.31070(13) 0.0836(6) Uani 1 2 d DS TU P C .
P1_2 P 0.42568(6) 0.32070(14) 0.4321(2) 0.0992(9) Uani 1 1 d D U . . .
C1_2 C 0.5070(5) 0.3172(9) 0.2445(18) 0.069(4) Uani 0.5 1 d D U P C -1
H1A_2 H 0.5078 0.3294 0.1400 0.083 Uiso 0.5 1 calc R U P C -1
H1B_2 H 0.5137 0.3509 0.3140 0.083 Uiso 0.5 1 calc R U P C -1
C2_2 C 0.5215(3) 0.2561(16) 0.2811(11) 0.065(4) Uani 0.5 1 d D U P C -1
H2_2 H 0.5414 0.2494 0.3646 0.077 Uiso 0.5 1 calc R U P C -1
C3_2 C 0.5050(5) 0.2068(9) 0.2053(16) 0.069(4) Uani 0.5 1 d D U P C -1
H3_2 H 0.5125 0.1654 0.2462 0.082 Uiso 0.5 1 calc R U P C -1
C4_2 C 0.4924(3) 0.2063(7) 0.0480(12) 0.071(4) Uani 0.5 1 d D U P C -1
H4A_2 H 0.4939 0.1631 0.0129 0.086 Uiso 0.5 1 calc R U P C -1
H4B_2 H 0.5138 0.2302 -0.0073 0.086 Uiso 0.5 1 calc R U P C -1
C5_2 C 0.4493(3) 0.2314(8) 0.0082(13) 0.075(5) Uani 0.5 1 d D U P C -1
O5_2 O 0.4319(2) 0.2664(6) 0.1023(8) 0.075(4) Uani 0.5 1 d D U P C -1
O6_2 O 0.4337(3) 0.2168(6) -0.1099(10) 0.113(5) Uani 0.5 1 d D U P C -1
C10_2 C 0.3819(4) 0.2695(8) 0.5318(15) 0.086(4) Uani 0.5 1 d D U P D -1
H10A_2 H 0.3719 0.2924 0.6190 0.103 Uiso 0.5 1 calc R U P D -1
H10B_2 H 0.3576 0.2651 0.4645 0.103 Uiso 0.5 1 calc R U P D -1
C9_2 C 0.3952(4) 0.2061(8) 0.5799(15) 0.073(4) Uani 0.5 1 d D U P . .
H9A_2 H 0.3704 0.1792 0.5966 0.087 Uiso 0.5 1 calc R U P D .
H9B_2 H 0.4122 0.2079 0.6709 0.087 Uiso 0.5 1 calc R U P . .
C11_2 C 0.39178(19) 0.3743(4) 0.3280(8) 0.089(2) Uani 1 1 d D U . . .
H11_2 H 0.3763 0.4007 0.4001 0.107 Uiso 1 1 calc R U . . .
C12_2 C 0.4183(2) 0.4168(4) 0.2311(8) 0.082(2) Uani 1 1 d D U . . .
H12A_2 H 0.4362 0.3914 0.1657 0.098 Uiso 1 1 calc R U . . .
H12B_2 H 0.4373 0.4418 0.2939 0.098 Uiso 1 1 calc R U . . .
C13_2 C 0.3909(2) 0.4605(4) 0.1374(9) 0.093(3) Uani 1 1 d D U . . .
H13A_2 H 0.3759 0.4900 0.2020 0.112 Uiso 1 1 calc R U . . .
H13B_2 H 0.4092 0.4845 0.0705 0.112 Uiso 1 1 calc R U . . .
C14_2 C 0.3590(2) 0.4243(4) 0.0489(10) 0.092(3) Uani 1 1 d D U . . .
H14A_2 H 0.3410 0.4533 -0.0068 0.111 Uiso 1 1 calc R U . . .
H14B_2 H 0.3741 0.3978 -0.0224 0.111 Uiso 1 1 calc R U . . .
C15_2 C 0.3315(2) 0.3844(4) 0.1454(10) 0.098(3) Uani 1 1 d D U . . .
H15A_2 H 0.3118 0.3600 0.0840 0.118 Uiso 1 1 calc R U . . .
H15B_2 H 0.3145 0.4108 0.2114 0.118 Uiso 1 1 calc R U . . .
C16_2 C 0.3591(2) 0.3406(4) 0.2364(10) 0.102(3) Uani 1 1 d D U . . .
H16A_2 H 0.3407 0.3160 0.3020 0.122 Uiso 1 1 calc R U . . .
H16B_2 H 0.3738 0.3116 0.1697 0.122 Uiso 1 1 calc R U . . .
C21_2 C 0.4575(2) 0.3731(5) 0.5517(9) 0.129(3) Uani 1 1 d D U . . .
H21_2 H 0.4732 0.4001 0.4814 0.154 Uiso 1 1 calc R U . . .
C22_2 C 0.4313(3) 0.4185(6) 0.6445(11) 0.149(4) Uani 1 1 d D U . . .
H22A_2 H 0.4128 0.3950 0.7122 0.179 Uiso 1 1 calc R U . . .
H22B_2 H 0.4130 0.4434 0.5794 0.179 Uiso 1 1 calc R U . . .
C23_2 C 0.4604(4) 0.4619(7) 0.7338(16) 0.214(6) Uani 1 1 d D U . . .
H23A_2 H 0.4741 0.4912 0.6652 0.257 Uiso 1 1 calc R U . . .
H23B_2 H 0.4426 0.4864 0.8013 0.257 Uiso 1 1 calc R U . . .
C24_2 C 0.4929(4) 0.4321(8) 0.8184(14) 0.221(7) Uani 1 1 d D U . . .
H24A_2 H 0.4799 0.4094 0.9010 0.265 Uiso 1 1 calc R U . . .
H24B_2 H 0.5122 0.4637 0.8596 0.265 Uiso 1 1 calc R U . . .
C25_2 C 0.5184(3) 0.3870(7) 0.7242(12) 0.198(6) Uani 1 1 d D U . . .
H25A_2 H 0.5361 0.4108 0.6550 0.237 Uiso 1 1 calc R U . . .
H25B_2 H 0.5375 0.3629 0.7883 0.237 Uiso 1 1 calc R U . . .
C26_2 C 0.4909(3) 0.3430(6) 0.6388(11) 0.183(5) Uani 1 1 d D U . . .
H26A_2 H 0.5091 0.3187 0.5721 0.219 Uiso 1 1 calc R U . . .
H26B_2 H 0.4775 0.3138 0.7081 0.219 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C3_1 Ni1_1 C2_1 39.9(6) . .
C3_1 Ni1_1 O5_1 86.0(4) . .
C2_1 Ni1_1 O5_1 105.4(4) . .
C3_1 Ni1_1 P1_1 109.0(4) . 7_575
C2_1 Ni1_1 P1_1 127.6(7) . 7_575
O5_1 Ni1_1 P1_1 113.7(2) . 7_575
C3_1 Ni1_1 P1_1 158.0(4) . .
C2_1 Ni1_1 P1_1 118.9(7) . .
O5_1 Ni1_1 P1_1 98.0(2) . .
P1_1 Ni1_1 P1_1 89.20(11) 7_575 .
C3_1 Ni1_1 C1_1 70.2(6) . .
C2_1 Ni1_1 C1_1 39.5(8) . .
O5_1 Ni1_1 C1_1 86.6(4) . .
P1_1 Ni1_1 C1_1 159.7(4) 7_575 .
P1_1 Ni1_1 C1_1 88.4(4) . .
C9_1 P1_1 C11_1 108.4(7) 7_575 .
C9_1 P1_1 C21_1 94.8(6) 7_575 .
C11_1 P1_1 C21_1 104.1(4) . .
C9_1 P1_1 C10_1 19.5(7) 7_575 .
C11_1 P1_1 C10_1 99.8(6) . .
C21_1 P1_1 C10_1 114.1(6) . .
C9_1 P1_1 Ni1_1 113.3(6) 7_575 .
C11_1 P1_1 Ni1_1 117.0(3) . .
C21_1 P1_1 Ni1_1 116.7(3) . .
C10_1 P1_1 Ni1_1 104.2(4) . .
C2_1 C1_1 Ni1_1 63.2(6) . .
C2_1 C1_1 H1A_1 117.4 . .
Ni1_1 C1_1 H1A_1 117.4 . .
C2_1 C1_1 H1B_1 117.4 . .
Ni1_1 C1_1 H1B_1 117.4 . .
H1A_1 C1_1 H1B_1 114.5 . .
C3_1 C2_1 C1_1 119.5(12) . .
C3_1 C2_1 Ni1_1 69.9(7) . .
C1_1 C2_1 Ni1_1 77.3(8) . .
C3_1 C2_1 H2_1 120.2 . .
C1_1 C2_1 H2_1 120.2 . .
Ni1_1 C2_1 H2_1 120.2 . .
C2_1 C3_1 C4_1 125.0(14) . .
C2_1 C3_1 Ni1_1 70.1(7) . .
C4_1 C3_1 Ni1_1 105.7(8) . .
C2_1 C3_1 H3_1 115.3 . .
C4_1 C3_1 H3_1 115.3 . .
Ni1_1 C3_1 H3_1 115.3 . .
C3_1 C4_1 C5_1 117.2(10) . .
C3_1 C4_1 H4A_1 108.0 . .
C5_1 C4_1 H4A_1 108.0 . .
C3_1 C4_1 H4B_1 108.0 . .
C5_1 C4_1 H4B_1 108.0 . .
H4A_1 C4_1 H4B_1 107.2 . .
O6_1 C5_1 O5_1 126.1(12) . .
O6_1 C5_1 C4_1 118.0(12) . .
O5_1 C5_1 C4_1 115.9(9) . .
C5_1 O5_1 Ni1_1 110.6(7) . .
C9_1 C10_1 P1_1 113.3(13) . .
C9_1 C10_1 H10A_1 108.9 . .
P1_1 C10_1 H10A_1 108.9 . .
C9_1 C10_1 H10B_1 108.9 . .
P1_1 C10_1 H10B_1 108.9 . .
H10A_1 C10_1 H10B_1 107.7 . .
C10_1 C9_1 P1_1 108.0(13) . 7_575
C10_1 C9_1 H9A_1 110.1 . .
P1_1 C9_1 H9A_1 110.1 7_575 .
C10_1 C9_1 H9B_1 110.1 . .
P1_1 C9_1 H9B_1 110.1 7_575 .
H9A_1 C9_1 H9B_1 108.4 . .
C12_1 C11_1 C16_1 109.7(7) . .
C12_1 C11_1 P1_1 109.7(4) . .
C16_1 C11_1 P1_1 111.7(5) . .
C12_1 C11_1 H11_1 108.5 . .
C16_1 C11_1 H11_1 108.5 . .
P1_1 C11_1 H11_1 108.5 . .
C11_1 C12_1 C13_1 111.4(6) . .
C11_1 C12_1 H12A_1 109.3 . .
C13_1 C12_1 H12A_1 109.3 . .
C11_1 C12_1 H12B_1 109.3 . .
C13_1 C12_1 H12B_1 109.3 . .
H12A_1 C12_1 H12B_1 108.0 . .
C14_1 C13_1 C12_1 109.4(7) . .
C14_1 C13_1 H13A_1 109.8 . .
C12_1 C13_1 H13A_1 109.8 . .
C14_1 C13_1 H13B_1 109.8 . .
C12_1 C13_1 H13B_1 109.8 . .
H13A_1 C13_1 H13B_1 108.2 . .
C15_1 C14_1 C13_1 110.9(8) . .
C15_1 C14_1 H14A_1 109.5 . .
C13_1 C14_1 H14A_1 109.5 . .
C15_1 C14_1 H14B_1 109.5 . .
C13_1 C14_1 H14B_1 109.5 . .
H14A_1 C14_1 H14B_1 108.0 . .
C14_1 C15_1 C16_1 110.7(7) . .
C14_1 C15_1 H15A_1 109.5 . .
C16_1 C15_1 H15A_1 109.5 . .
C14_1 C15_1 H15B_1 109.5 . .
C16_1 C15_1 H15B_1 109.5 . .
H15A_1 C15_1 H15B_1 108.1 . .
C11_1 C16_1 C15_1 111.0(6) . .
C11_1 C16_1 H16A_1 109.4 . .
C15_1 C16_1 H16A_1 109.4 . .
C11_1 C16_1 H16B_1 109.4 . .
C15_1 C16_1 H16B_1 109.4 . .
H16A_1 C16_1 H16B_1 108.0 . .
C26_1 C21_1 C22_1 111.6(7) . .
C26_1 C21_1 P1_1 113.0(6) . .
C22_1 C21_1 P1_1 113.9(6) . .
C26_1 C21_1 H21_1 105.9 . .
C22_1 C21_1 H21_1 105.9 . .
P1_1 C21_1 H21_1 105.9 . .
C21_1 C22_1 C23_1 110.5(8) . .
C21_1 C22_1 H22A_1 109.5 . .
C23_1 C22_1 H22A_1 109.5 . .
C21_1 C22_1 H22B_1 109.5 . .
C23_1 C22_1 H22B_1 109.5 . .
H22A_1 C22_1 H22B_1 108.1 . .
C24_1 C23_1 C22_1 113.5(10) . .
C24_1 C23_1 H23A_1 108.9 . .
C22_1 C23_1 H23A_1 108.9 . .
C24_1 C23_1 H23B_1 108.9 . .
C22_1 C23_1 H23B_1 108.9 . .
H23A_1 C23_1 H23B_1 107.7 . .
C23_1 C24_1 C25_1 113.0(10) . .
C23_1 C24_1 H24A_1 109.0 . .
C25_1 C24_1 H24A_1 109.0 . .
C23_1 C24_1 H24B_1 109.0 . .
C25_1 C24_1 H24B_1 109.0 . .
H24A_1 C24_1 H24B_1 107.8 . .
C26_1 C25_1 C24_1 112.0(9) . .
C26_1 C25_1 H25A_1 109.2 . .
C24_1 C25_1 H25A_1 109.2 . .
C26_1 C25_1 H25B_1 109.2 . .
C24_1 C25_1 H25B_1 109.2 . .
H25A_1 C25_1 H25B_1 107.9 . .
C21_1 C26_1 C25_1 112.2(8) . .
C21_1 C26_1 H26A_1 109.2 . .
C25_1 C26_1 H26A_1 109.2 . .
C21_1 C26_1 H26B_1 109.2 . .
C25_1 C26_1 H26B_1 109.2 . .
H26A_1 C26_1 H26B_1 107.9 . .
C3_2 Ni1_2 C2_2 40.5(7) . .
C3_2 Ni1_2 O5_2 86.6(5) . .
C2_2 Ni1_2 O5_2 105.7(4) . .
C3_2 Ni1_2 P1_2 105.9(6) . 7_565
C2_2 Ni1_2 P1_2 126.9(9) . 7_565
O5_2 Ni1_2 P1_2 112.2(3) . 7_565
C3_2 Ni1_2 P1_2 160.6(6) . .
C2_2 Ni1_2 P1_2 120.5(9) . .
O5_2 Ni1_2 P1_2 98.1(3) . .
P1_2 Ni1_2 P1_2 89.83(15) 7_565 .
C3_2 Ni1_2 C1_2 70.9(6) . .
C2_2 Ni1_2 C1_2 40.0(8) . .
O5_2 Ni1_2 C1_2 85.6(5) . .
P1_2 Ni1_2 C1_2 162.0(5) 7_565 .
P1_2 Ni1_2 C1_2 90.6(5) . .
C9_2 P1_2 C11_2 106.5(6) 7_565 .
C9_2 P1_2 C21_2 92.7(5) 7_565 .
C11_2 P1_2 C21_2 103.5(4) . .
C9_2 P1_2 C10_2 23.8(6) 7_565 .
C11_2 P1_2 C10_2 100.4(5) . .
C21_2 P1_2 C10_2 116.4(5) . .
C9_2 P1_2 Ni1_2 115.4(6) 7_565 .
C11_2 P1_2 Ni1_2 117.7(3) . .
C21_2 P1_2 Ni1_2 117.6(3) . .
C10_2 P1_2 Ni1_2 100.4(5) . .
C2_2 C1_2 Ni1_2 62.8(7) . .
C2_2 C1_2 H1A_2 117.5 . .
Ni1_2 C1_2 H1A_2 117.5 . .
C2_2 C1_2 H1B_2 117.5 . .
Ni1_2 C1_2 H1B_2 117.5 . .
H1A_2 C1_2 H1B_2 114.6 . .
C3_2 C2_2 C1_2 118.4(12) . .
C3_2 C2_2 Ni1_2 69.0(8) . .
C1_2 C2_2 Ni1_2 77.2(9) . .
C3_2 C2_2 H2_2 120.7 . .
C1_2 C2_2 H2_2 120.7 . .
Ni1_2 C2_2 H2_2 120.7 . .
C2_2 C3_2 C4_2 126.3(15) . .
C2_2 C3_2 Ni1_2 70.5(7) . .
C4_2 C3_2 Ni1_2 106.1(9) . .
C2_2 C3_2 H3_2 114.7 . .
C4_2 C3_2 H3_2 114.7 . .
Ni1_2 C3_2 H3_2 114.7 . .
C3_2 C4_2 C5_2 118.0(10) . .
C3_2 C4_2 H4A_2 107.8 . .
C5_2 C4_2 H4A_2 107.8 . .
C3_2 C4_2 H4B_2 107.8 . .
C5_2 C4_2 H4B_2 107.8 . .
H4A_2 C4_2 H4B_2 107.1 . .
O6_2 C5_2 O5_2 125.1(12) . .
O6_2 C5_2 C4_2 118.7(12) . .
O5_2 C5_2 C4_2 116.3(10) . .
C5_2 O5_2 Ni1_2 109.3(8) . .
C9_2 C10_2 P1_2 116.6(11) . .
C9_2 C10_2 H10A_2 108.1 . .
P1_2 C10_2 H10A_2 108.1 . .
C9_2 C10_2 H10B_2 108.1 . .
P1_2 C10_2 H10B_2 108.1 . .
H10A_2 C10_2 H10B_2 107.3 . .
C10_2 C9_2 P1_2 103.3(10) . 7_565
C10_2 C9_2 H9A_2 111.1 . .
P1_2 C9_2 H9A_2 111.1 7_565 .
C10_2 C9_2 H9B_2 111.1 . .
P1_2 C9_2 H9B_2 111.1 7_565 .
H9A_2 C9_2 H9B_2 109.1 . .
C16_2 C11_2 C12_2 110.2(6) . .
C16_2 C11_2 P1_2 112.3(6) . .
C12_2 C11_2 P1_2 110.9(4) . .
C16_2 C11_2 H11_2 107.7 . .
C12_2 C11_2 H11_2 107.7 . .
P1_2 C11_2 H11_2 107.7 . .
C11_2 C12_2 C13_2 112.4(6) . .
C11_2 C12_2 H12A_2 109.1 . .
C13_2 C12_2 H12A_2 109.1 . .
C11_2 C12_2 H12B_2 109.1 . .
C13_2 C12_2 H12B_2 109.1 . .
H12A_2 C12_2 H12B_2 107.9 . .
C14_2 C13_2 C12_2 110.8(7) . .
C14_2 C13_2 H13A_2 109.5 . .
C12_2 C13_2 H13A_2 109.5 . .
C14_2 C13_2 H13B_2 109.5 . .
C12_2 C13_2 H13B_2 109.5 . .
H13A_2 C13_2 H13B_2 108.1 . .
C15_2 C14_2 C13_2 111.7(7) . .
C15_2 C14_2 H14A_2 109.3 . .
C13_2 C14_2 H14A_2 109.3 . .
C15_2 C14_2 H14B_2 109.3 . .
C13_2 C14_2 H14B_2 109.3 . .
H14A_2 C14_2 H14B_2 107.9 . .
C14_2 C15_2 C16_2 109.9(6) . .
C14_2 C15_2 H15A_2 109.7 . .
C16_2 C15_2 H15A_2 109.7 . .
C14_2 C15_2 H15B_2 109.7 . .
C16_2 C15_2 H15B_2 109.7 . .
H15A_2 C15_2 H15B_2 108.2 . .
C11_2 C16_2 C15_2 113.0(7) . .
C11_2 C16_2 H16A_2 109.0 . .
C15_2 C16_2 H16A_2 109.0 . .
C11_2 C16_2 H16B_2 109.0 . .
C15_2 C16_2 H16B_2 109.0 . .
H16A_2 C16_2 H16B_2 107.8 . .
C26_2 C21_2 C22_2 111.8(7) . .
C26_2 C21_2 P1_2 115.7(8) . .
C22_2 C21_2 P1_2 114.7(6) . .
C26_2 C21_2 H21_2 104.3 . .
C22_2 C21_2 H21_2 104.3 . .
P1_2 C21_2 H21_2 104.3 . .
C21_2 C22_2 C23_2 110.9(8) . .
C21_2 C22_2 H22A_2 109.5 . .
C23_2 C22_2 H22A_2 109.5 . .
C21_2 C22_2 H22B_2 109.5 . .
C23_2 C22_2 H22B_2 109.5 . .
H22A_2 C22_2 H22B_2 108.1 . .
C24_2 C23_2 C22_2 115.8(13) . .
C24_2 C23_2 H23A_2 108.3 . .
C22_2 C23_2 H23A_2 108.3 . .
C24_2 C23_2 H23B_2 108.3 . .
C22_2 C23_2 H23B_2 108.3 . .
H23A_2 C23_2 H23B_2 107.4 . .
C23_2 C24_2 C25_2 111.2(10) . .
C23_2 C24_2 H24A_2 109.4 . .
C25_2 C24_2 H24A_2 109.4 . .
C23_2 C24_2 H24B_2 109.4 . .
C25_2 C24_2 H24B_2 109.4 . .
H24A_2 C24_2 H24B_2 108.0 . .
C26_2 C25_2 C24_2 113.0(9) . .
C26_2 C25_2 H25A_2 109.0 . .
C24_2 C25_2 H25A_2 109.0 . .
C26_2 C25_2 H25B_2 109.0 . .
C24_2 C25_2 H25B_2 109.0 . .
H25A_2 C25_2 H25B_2 107.8 . .
C21_2 C26_2 C25_2 114.4(11) . .
C21_2 C26_2 H26A_2 108.7 . .
C25_2 C26_2 H26A_2 108.7 . .
C21_2 C26_2 H26B_2 108.7 . .
C25_2 C26_2 H26B_2 108.7 . .
H26A_2 C26_2 H26B_2 107.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1_1 C3_1 2.001(12) .
Ni1_1 C2_1 2.003(8) .
Ni1_1 O5_1 2.115(7) .
Ni1_1 P1_1 2.149(2) 7_575
Ni1_1 P1_1 2.149(2) .
Ni1_1 C1_1 2.191(13) .
P1_1 C9_1 1.757(16) 7_575
P1_1 C11_1 1.855(6) .
P1_1 C21_1 1.857(8) .
P1_1 C10_1 1.949(13) .
C1_1 C2_1 1.43(3) .
C1_1 H1A_1 0.9900 .
C1_1 H1B_1 0.9900 .
C2_1 C3_1 1.37(2) .
C2_1 H2_1 1.0000 .
C3_1 C4_1 1.506(15) .
C3_1 H3_1 1.0000 .
C4_1 C5_1 1.520(15) .
C4_1 H4A_1 0.9900 .
C4_1 H4B_1 0.9900 .
C5_1 O6_1 1.224(12) .
C5_1 O5_1 1.254(14) .
C10_1 C9_1 1.487(15) .
C10_1 H10A_1 0.9900 .
C10_1 H10B_1 0.9900 .
C9_1 P1_1 1.757(16) 7_575
C9_1 H9A_1 0.9900 .
C9_1 H9B_1 0.9900 .
C11_1 C12_1 1.522(9) .
C11_1 C16_1 1.524(9) .
C11_1 H11_1 1.0000 .
C12_1 C13_1 1.544(9) .
C12_1 H12A_1 0.9900 .
C12_1 H12B_1 0.9900 .
C13_1 C14_1 1.520(11) .
C13_1 H13A_1 0.9900 .
C13_1 H13B_1 0.9900 .
C14_1 C15_1 1.517(11) .
C14_1 H14A_1 0.9900 .
C14_1 H14B_1 0.9900 .
C15_1 C16_1 1.532(9) .
C15_1 H15A_1 0.9900 .
C15_1 H15B_1 0.9900 .
C16_1 H16A_1 0.9900 .
C16_1 H16B_1 0.9900 .
C21_1 C26_1 1.501(10) .
C21_1 C22_1 1.525(10) .
C21_1 H21_1 1.0000 .
C22_1 C23_1 1.557(12) .
C22_1 H22A_1 0.9900 .
C22_1 H22B_1 0.9900 .
C23_1 C24_1 1.440(13) .
C23_1 H23A_1 0.9900 .
C23_1 H23B_1 0.9900 .
C24_1 C25_1 1.527(12) .
C24_1 H24A_1 0.9900 .
C24_1 H24B_1 0.9900 .
C25_1 C26_1 1.505(11) .
C25_1 H25A_1 0.9900 .
C25_1 H25B_1 0.9900 .
C26_1 H26A_1 0.9900 .
C26_1 H26B_1 0.9900 .
Ni1_2 C3_2 1.973(14) .
Ni1_2 C2_2 1.992(8) .
Ni1_2 O5_2 2.120(7) .
Ni1_2 P1_2 2.167(3) 7_565
Ni1_2 P1_2 2.167(3) .
Ni1_2 C1_2 2.183(15) .
P1_2 C9_2 1.756(15) 7_565
P1_2 C11_2 1.843(7) .
P1_2 C21_2 1.868(9) .
P1_2 C10_2 1.993(13) .
C1_2 C2_2 1.44(3) .
C1_2 H1A_2 0.9900 .
C1_2 H1B_2 0.9900 .
C2_2 C3_2 1.37(2) .
C2_2 H2_2 1.0000 .
C3_2 C4_2 1.490(17) .
C3_2 H3_2 1.0000 .
C4_2 C5_2 1.513(15) .
C4_2 H4A_2 0.9900 .
C4_2 H4B_2 0.9900 .
C5_2 O6_2 1.227(12) .
C5_2 O5_2 1.270(14) .
C10_2 C9_2 1.502(16) .
C10_2 H10A_2 0.9900 .
C10_2 H10B_2 0.9900 .
C9_2 P1_2 1.756(15) 7_565
C9_2 H9A_2 0.9900 .
C9_2 H9B_2 0.9900 .
C11_2 C16_2 1.515(10) .
C11_2 C12_2 1.528(9) .
C11_2 H11_2 1.0000 .
C12_2 C13_2 1.543(9) .
C12_2 H12A_2 0.9900 .
C12_2 H12B_2 0.9900 .
C13_2 C14_2 1.511(9) .
C13_2 H13A_2 0.9900 .
C13_2 H13B_2 0.9900 .
C14_2 C15_2 1.510(10) .
C14_2 H14A_2 0.9900 .
C14_2 H14B_2 0.9900 .
C15_2 C16_2 1.533(9) .
C15_2 H15A_2 0.9900 .
C15_2 H15B_2 0.9900 .
C16_2 H16A_2 0.9900 .
C16_2 H16B_2 0.9900 .
C21_2 C26_2 1.475(11) .
C21_2 C22_2 1.540(11) .
C21_2 H21_2 1.0000 .
C22_2 C23_2 1.549(13) .
C22_2 H22A_2 0.9900 .
C22_2 H22B_2 0.9900 .
C23_2 C24_2 1.440(14) .
C23_2 H23A_2 0.9900 .
C23_2 H23B_2 0.9900 .
C24_2 C25_2 1.529(12) .
C24_2 H24A_2 0.9900 .
C24_2 H24B_2 0.9900 .
C25_2 C26_2 1.506(13) .
C25_2 H25A_2 0.9900 .
C25_2 H25B_2 0.9900 .
C26_2 H26A_2 0.9900 .
C26_2 H26B_2 0.9900 .
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_4
Ni1_1 C1_1 C2_1 C3_1 57.9(9) . .
C1_1 C2_1 C3_1 C4_1 33.9(15) . .
Ni1_1 C2_1 C3_1 C4_1 95.6(12) . .
C1_1 C2_1 C3_1 Ni1_1 -61.7(9) . .
C2_1 C3_1 C4_1 C5_1 -85.2(17) . .
Ni1_1 C3_1 C4_1 C5_1 -8.8(16) . .
C3_1 C4_1 C5_1 O6_1 -157.7(14) . .
C3_1 C4_1 C5_1 O5_1 23(2) . .
O6_1 C5_1 O5_1 Ni1_1 157.5(13) . .
C4_1 C5_1 O5_1 Ni1_1 -23.4(15) . .
P1_1 C10_1 C9_1 P1_1 -37.8(18) . 7_575
C9_1 P1_1 C11_1 C12_1 166.2(7) 7_575 .
C21_1 P1_1 C11_1 C12_1 66.2(7) . .
C10_1 P1_1 C11_1 C12_1 -175.8(7) . .
Ni1_1 P1_1 C11_1 C12_1 -64.2(6) . .
C9_1 P1_1 C11_1 C16_1 -71.9(8) 7_575 .
C21_1 P1_1 C11_1 C16_1 -171.9(6) . .
C10_1 P1_1 C11_1 C16_1 -53.9(8) . .
Ni1_1 P1_1 C11_1 C16_1 57.7(6) . .
C16_1 C11_1 C12_1 C13_1 57.3(9) . .
P1_1 C11_1 C12_1 C13_1 -179.6(6) . .
C11_1 C12_1 C13_1 C14_1 -57.7(11) . .
C12_1 C13_1 C14_1 C15_1 57.3(11) . .
C13_1 C14_1 C15_1 C16_1 -57.6(11) . .
C12_1 C11_1 C16_1 C15_1 -56.7(9) . .
P1_1 C11_1 C16_1 C15_1 -178.6(6) . .
C14_1 C15_1 C16_1 C11_1 57.1(11) . .
C9_1 P1_1 C21_1 C26_1 75.2(10) 7_575 .
C11_1 P1_1 C21_1 C26_1 -174.5(7) . .
C10_1 P1_1 C21_1 C26_1 77.7(9) . .
Ni1_1 P1_1 C21_1 C26_1 -44.0(8) . .
C9_1 P1_1 C21_1 C22_1 -53.5(10) 7_575 .
C11_1 P1_1 C21_1 C22_1 56.8(8) . .
C10_1 P1_1 C21_1 C22_1 -51.0(9) . .
Ni1_1 P1_1 C21_1 C22_1 -172.7(6) . .
C26_1 C21_1 C22_1 C23_1 52.6(12) . .
P1_1 C21_1 C22_1 C23_1 -178.0(9) . .
C21_1 C22_1 C23_1 C24_1 -52.2(16) . .
C22_1 C23_1 C24_1 C25_1 51.8(18) . .
C23_1 C24_1 C25_1 C26_1 -52.2(17) . .
C22_1 C21_1 C26_1 C25_1 -54.7(12) . .
P1_1 C21_1 C26_1 C25_1 175.4(7) . .
C24_1 C25_1 C26_1 C21_1 53.3(14) . .
Ni1_2 C1_2 C2_2 C3_2 57.2(9) . .
C1_2 C2_2 C3_2 C4_2 34.5(15) . .
Ni1_2 C2_2 C3_2 C4_2 96.0(13) . .
C1_2 C2_2 C3_2 Ni1_2 -61.4(9) . .
C2_2 C3_2 C4_2 C5_2 -82.4(19) . .
Ni1_2 C3_2 C4_2 C5_2 -5.2(18) . .
C3_2 C4_2 C5_2 O6_2 -160.5(15) . .
C3_2 C4_2 C5_2 O5_2 19(2) . .
O6_2 C5_2 O5_2 Ni1_2 158.6(14) . .
C4_2 C5_2 O5_2 Ni1_2 -21.1(15) . .
P1_2 C10_2 C9_2 P1_2 -41.6(11) . 7_565
C9_2 P1_2 C11_2 C16_2 -75.9(8) 7_565 .
C21_2 P1_2 C11_2 C16_2 -172.8(6) . .
C10_2 P1_2 C11_2 C16_2 -52.2(7) . .
Ni1_2 P1_2 C11_2 C16_2 55.5(6) . .
C9_2 P1_2 C11_2 C12_2 160.3(7) 7_565 .
C21_2 P1_2 C11_2 C12_2 63.4(7) . .
C10_2 P1_2 C11_2 C12_2 -176.0(7) . .
Ni1_2 P1_2 C11_2 C12_2 -68.3(6) . .
C16_2 C11_2 C12_2 C13_2 52.6(9) . .
P1_2 C11_2 C12_2 C13_2 177.6(6) . .
C11_2 C12_2 C13_2 C14_2 -54.3(9) . .
C12_2 C13_2 C14_2 C15_2 56.4(9) . .
C13_2 C14_2 C15_2 C16_2 -57.0(10) . .
C12_2 C11_2 C16_2 C15_2 -54.0(9) . .
P1_2 C11_2 C16_2 C15_2 -178.2(6) . .
C14_2 C15_2 C16_2 C11_2 56.3(10) . .
C9_2 P1_2 C21_2 C26_2 78.0(9) 7_565 .
C11_2 P1_2 C21_2 C26_2 -174.3(7) . .
C10_2 P1_2 C21_2 C26_2 76.6(9) . .
Ni1_2 P1_2 C21_2 C26_2 -42.6(9) . .
C9_2 P1_2 C21_2 C22_2 -54.5(10) 7_565 .
C11_2 P1_2 C21_2 C22_2 53.2(9) . .
C10_2 P1_2 C21_2 C22_2 -55.9(10) . .
Ni1_2 P1_2 C21_2 C22_2 -175.1(7) . .
C26_2 C21_2 C22_2 C23_2 48.5(15) . .
P1_2 C21_2 C22_2 C23_2 -177.2(9) . .
C21_2 C22_2 C23_2 C24_2 -50.8(16) . .
C22_2 C23_2 C24_2 C25_2 51.1(19) . .
C23_2 C24_2 C25_2 C26_2 -50.4(19) . .
C22_2 C21_2 C26_2 C25_2 -51.1(14) . .
P1_2 C21_2 C26_2 C25_2 175.1(8) . .
C24_2 C25_2 C26_2 C21_2 51.9(16) . .
