#------------------------------------------------------------------------------
#$Date: 2022-02-04 04:17:45 +0200 (Fri, 04 Feb 2022) $
#$Revision: 272545 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/43/7244346.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_7244346
loop_
_publ_author_name
'Panigrahi, Dipankar'
'Mondal, Munmun'
'Gupta, Rohit'
'Mani, Ganesan'
_publ_section_title
;
 Four- and five-coordinate nickel(ii) complexes bearing new
 diphosphine--phosphonite and triphosphine--phosphite ligands: catalysts
 for N-alkylation of amines
;
_journal_issue                   8
_journal_name_full               'RSC Advances'
_journal_page_first              4510
_journal_page_last               4520
_journal_paper_doi               10.1039/D1RA08961G
_journal_volume                  12
_journal_year                    2022
_chemical_formula_sum            'C43 H49 Cl2 F12 N2 Ni O2 P5'
_chemical_formula_weight         1138.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-12-09 deposited with the CCDC.	2021-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.139(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.235(2)
_cell_length_b                   22.991(4)
_cell_length_c                   20.206(4)
_cell_measurement_reflns_used    105309
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.997
_cell_measurement_theta_min      2.216
_cell_volume                     5178.8(16)
_computing_molecular_graphics    ortep
_computing_publication_material  ciftab
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'APEX3 D8 QUEST PHOTON-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0911
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            105309
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.216
_diffrn_source                   'Fine focused sealed tube'
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       needle
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.090
_exptl_transmission_factor_max   0.7455
_exptl_transmission_factor_min   0.6925
_refine_diff_density_max         1.079
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         9088
_refine_ls_number_restraints     197
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0658
_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)+(0.1160P)²+3.3924P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1895
_refine_ls_wR_factor_ref         0.2038
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6270
_reflns_number_total             9088
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ra08961g2.cif
_cod_data_source_block           LNiCNBu2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7244346
_shelx_shelxl_version_number     2018/3
_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   0.882
_shelx_estimated_absorpt_t_max   0.939
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 Ni -0.00869(4) -0.25780(2) 0.58864(3) 0.04575(19) Uani 1 1 d . . . . .
P5 P 0.14415(9) -0.29086(5) 0.65226(6) 0.0504(3) Uani 1 1 d . . . . .
P4 P -0.11488(9) -0.29712(5) 0.66314(5) 0.0501(3) Uani 1 1 d . . . . .
P3 P 0.09627(10) -0.17576(4) 0.58939(6) 0.0525(3) Uani 1 1 d . . . . .
O1 O 0.1091(3) -0.31383(14) 0.72167(15) 0.0671(8) Uani 1 1 d . . . . .
O2 O 0.2445(3) -0.24253(12) 0.66935(17) 0.0668(9) Uani 1 1 d . . . . .
N2 N 0.0076(3) -0.34334(17) 0.4720(2) 0.0620(9) Uani 1 1 d . . . . .
N1 N -0.2367(4) -0.20346(17) 0.5224(2) 0.0699(11) Uani 1 1 d . . . . .
C38 C 0.0049(4) -0.31255(19) 0.5160(2) 0.0555(11) Uani 1 1 d . . . . .
C34 C -0.3563(4) -0.1816(2) 0.4954(3) 0.0801(15) Uani 1 1 d . . . . .
C33 C -0.1479(4) -0.22247(18) 0.5471(2) 0.0561(10) Uani 1 1 d . . . . .
C13 C -0.0085(4) -0.3033(2) 0.7405(2) 0.0614(11) Uani 1 1 d . . . . .
H13A H -0.008449 -0.267652 0.766150 0.074 Uiso 1 1 calc R U . . .
H13B H -0.031820 -0.335108 0.767646 0.074 Uiso 1 1 calc R U . . .
C23 C 0.3079(3) -0.09800(14) 0.4649(2) 0.0899(18) Uani 1 1 d G . . . .
H23 H 0.354195 -0.064437 0.465148 0.108 Uiso 1 1 calc R U . . .
C22 C 0.2483(3) -0.11110(13) 0.51937(18) 0.0752(14) Uani 1 1 d G . . . .
H22 H 0.254714 -0.086305 0.556006 0.090 Uiso 1 1 calc R U . . .
C21 C 0.1792(3) -0.16126(13) 0.51905(15) 0.0613(11) Uani 1 1 d G . . . .
C26 C 0.1697(3) -0.19832(13) 0.46429(18) 0.0883(17) Uani 1 1 d G . . . .
H26 H 0.123398 -0.231877 0.464076 0.106 Uiso 1 1 calc R U . . .
C25 C 0.2293(4) -0.18522(19) 0.40985(16) 0.112(2) Uani 1 1 d G . . . .
H25 H 0.222878 -0.210010 0.373218 0.134 Uiso 1 1 calc R U . . .
C24 C 0.2984(3) -0.1351(2) 0.41017(18) 0.098(2) Uani 1 1 d G . . . .
H24 H 0.338276 -0.126290 0.373753 0.117 Uiso 1 1 calc R U . . .
C39 C 0.0145(5) -0.3828(2) 0.4146(3) 0.0762(14) Uani 1 1 d . . . . .
C37 C -0.4472(5) -0.2210(3) 0.5213(3) 0.0970(18) Uani 1 1 d . . . . .
H37A H -0.439955 -0.259424 0.503731 0.146 Uiso 1 1 calc R U . . .
H37B H -0.526444 -0.206356 0.507569 0.146 Uiso 1 1 calc R U . . .
H37C H -0.433047 -0.222247 0.569134 0.146 Uiso 1 1 calc R U . . .
C20 C 0.2128(4) -0.18236(18) 0.6627(2) 0.0662(12) Uani 1 1 d . . . . .
H20A H 0.282552 -0.159258 0.655990 0.079 Uiso 1 1 calc R U . . .
H20B H 0.181790 -0.168668 0.702586 0.079 Uiso 1 1 calc R U . . .
C10 C -0.2888(3) -0.47327(11) 0.6042(2) 0.0883(17) Uani 1 1 d G . . . .
H10 H -0.327011 -0.508223 0.591911 0.106 Uiso 1 1 calc R U . . .
C11 C -0.2284(3) -0.46651(12) 0.66804(18) 0.0918(17) Uani 1 1 d G . . . .
H11 H -0.226203 -0.496932 0.698500 0.110 Uiso 1 1 calc R U . . .
C12 C -0.1713(3) -0.41427(14) 0.68637(13) 0.0766(14) Uani 1 1 d G . . . .
H12 H -0.130896 -0.409746 0.729102 0.092 Uiso 1 1 calc R U . . .
C7 C -0.1746(2) -0.36880(10) 0.64085(14) 0.0539(10) Uani 1 1 d G . . . .
C8 C -0.2350(3) -0.37556(11) 0.57699(13) 0.0666(12) Uani 1 1 d G . . . .
H8 H -0.237203 -0.345140 0.546527 0.080 Uiso 1 1 calc R U . . .
C9 C -0.2921(3) -0.42780(14) 0.55865(14) 0.0785(14) Uani 1 1 d G . . . .
H9 H -0.332511 -0.432326 0.515924 0.094 Uiso 1 1 calc R U . . .
C40 C 0.0049(9) -0.4434(3) 0.4421(4) 0.152(4) Uani 1 1 d . . . . .
H40A H 0.067961 -0.449460 0.478020 0.228 Uiso 1 1 calc R U . . .
H40B H 0.012012 -0.471298 0.407452 0.228 Uiso 1 1 calc R U . . .
H40C H -0.071407 -0.447908 0.458194 0.228 Uiso 1 1 calc R U . . .
C4 C -0.4305(3) -0.18919(19) 0.7196(2) 0.106(2) Uani 1 1 d G . . . .
H4 H -0.494377 -0.166810 0.730251 0.127 Uiso 1 1 calc R U . . .
C5 C -0.4442(2) -0.2489(2) 0.7106(2) 0.099(2) Uani 1 1 d G . . . .
H5 H -0.517303 -0.266400 0.715153 0.118 Uiso 1 1 calc R U . . .
C6 C -0.3487(3) -0.28229(13) 0.69467(19) 0.0787(14) Uani 1 1 d G . . . .
H6 H -0.357852 -0.322216 0.688614 0.094 Uiso 1 1 calc R U . . .
C1 C -0.2394(2) -0.25607(13) 0.68781(18) 0.0613(12) Uani 1 1 d G . . . .
C2 C -0.2257(3) -0.19640(14) 0.6969(2) 0.0883(17) Uani 1 1 d G . . . .
H2 H -0.152548 -0.178856 0.692270 0.106 Uiso 1 1 calc R U . . .
C3 C -0.3212(4) -0.16296(13) 0.7128(2) 0.114(2) Uani 1 1 d G . . . .
H3 H -0.311997 -0.123038 0.718809 0.137 Uiso 1 1 calc R U . . .
C35 C -0.3660(6) -0.1851(4) 0.4193(3) 0.124(3) Uani 1 1 d . . . . .
H35A H -0.347722 -0.223945 0.406299 0.186 Uiso 1 1 calc R U . . .
H35B H -0.310369 -0.158382 0.403428 0.186 Uiso 1 1 calc R U . . .
H35C H -0.446139 -0.175247 0.400390 0.186 Uiso 1 1 calc R U . . .
C41 C 0.1331(5) -0.3719(3) 0.3904(3) 0.103(2) Uani 1 1 d . . . . .
H41A H 0.136294 -0.332439 0.375095 0.154 Uiso 1 1 calc R U . . .
H41B H 0.142834 -0.397950 0.354335 0.154 Uiso 1 1 calc R U . . .
H41C H 0.196311 -0.378259 0.426198 0.154 Uiso 1 1 calc R U . . .
C17 C 0.3605(4) -0.44102(18) 0.5817(2) 0.128(3) Uani 1 1 d G . . . .
H17 H 0.404538 -0.471605 0.566949 0.154 Uiso 1 1 calc R U . . .
C18 C 0.3827(3) -0.3843(2) 0.56272(19) 0.113(2) Uani 1 1 d G . . . .
H18 H 0.441582 -0.376971 0.535288 0.136 Uiso 1 1 calc R U . . .
C19 C 0.3168(3) -0.33860(15) 0.58474(18) 0.0825(15) Uani 1 1 d G . . . .
H19 H 0.331667 -0.300666 0.572048 0.099 Uiso 1 1 calc R U . . .
C14 C 0.2288(3) -0.34958(11) 0.62573(17) 0.0608(11) Uani 1 1 d G . . . .
C15 C 0.2066(3) -0.40628(14) 0.6447(2) 0.0873(16) Uani 1 1 d G . . . .
H15 H 0.147661 -0.413626 0.672130 0.105 Uiso 1 1 calc R U . . .
C16 C 0.2724(4) -0.45200(11) 0.6227(3) 0.122(3) Uani 1 1 d G . . . .
H16 H 0.257575 -0.489932 0.635370 0.146 Uiso 1 1 calc R U . . .
C30 C -0.1229(4) -0.01166(14) 0.6182(2) 0.117(2) Uani 1 1 d G . . . .
H30 H -0.169759 0.020878 0.623863 0.141 Uiso 1 1 calc R U . . .
C31 C -0.0703(5) -0.04231(17) 0.67360(18) 0.138(3) Uani 1 1 d G . . . .
H31 H -0.082031 -0.030273 0.716255 0.166 Uiso 1 1 calc R U . . .
C32 C -0.0002(4) -0.09094(15) 0.66521(14) 0.100(2) Uani 1 1 d G . . . .
H32 H 0.034945 -0.111442 0.702245 0.119 Uiso 1 1 calc R U . . .
C27 C 0.0173(3) -0.10892(11) 0.60146(16) 0.0615(11) Uani 1 1 d G . . . .
C28 C -0.0353(3) -0.07828(14) 0.54610(14) 0.0745(14) Uani 1 1 d G . . . .
H28 H -0.023533 -0.090311 0.503448 0.089 Uiso 1 1 calc R U . . .
C29 C -0.1053(3) -0.02965(15) 0.55449(19) 0.0993(19) Uani 1 1 d G . . . .
H29 H -0.140510 -0.009141 0.517457 0.119 Uiso 1 1 calc R U . . .
C42 C -0.0882(6) -0.3658(4) 0.3625(3) 0.135(3) Uani 1 1 d . . . . .
H42A H -0.162952 -0.373070 0.379434 0.202 Uiso 1 1 calc R U . . .
H42B H -0.084509 -0.388276 0.322830 0.202 Uiso 1 1 calc R U . . .
H42C H -0.082282 -0.325166 0.352335 0.202 Uiso 1 1 calc R U . . .
C36 C -0.3634(6) -0.1191(3) 0.5194(5) 0.154(4) Uani 1 1 d . . . . .
H36A H -0.354603 -0.118460 0.567300 0.231 Uiso 1 1 calc R U . . .
H36B H -0.439664 -0.102804 0.502265 0.231 Uiso 1 1 calc R U . . .
H36C H -0.300359 -0.096682 0.503895 0.231 Uiso 1 1 calc R U . . .
P1 P -0.47845(13) -0.36698(6) 0.36612(7) 0.0761(4) Uani 1 1 d . . . . .
F6 F -0.3730(3) -0.34267(17) 0.4180(2) 0.1163(12) Uani 1 1 d . . . . .
F3 F -0.5852(4) -0.3913(2) 0.31618(19) 0.1291(14) Uani 1 1 d . . . . .
F1 F -0.4383(5) -0.32671(19) 0.3106(2) 0.1449(17) Uani 1 1 d . . . . .
F5 F -0.3944(4) -0.41535(18) 0.3432(3) 0.1461(16) Uani 1 1 d . . . . .
F4 F -0.5154(5) -0.4105(3) 0.4205(2) 0.162(2) Uani 1 1 d . . . . .
F2 F -0.5599(4) -0.3191(2) 0.3895(3) 0.183(3) Uani 1 1 d . . . . .
P2 P 0.06910(15) -0.50352(6) 0.82785(8) 0.0865(5) Uani 1 1 d DG U . . .
F11 F -0.0613(4) -0.5248(3) 0.7891(3) 0.179(4) Uani 0.573(4) 1 d DG U P A 1
F10 F 0.1152(6) -0.4886(3) 0.7556(2) 0.192(4) Uani 0.573(4) 1 d DG U P A 1
F9 F 0.1993(3) -0.4822(3) 0.8665(3) 0.167(3) Uani 0.573(4) 1 d DG U P A 1
F8 F 0.0227(6) -0.5183(3) 0.9001(2) 0.180(4) Uani 0.573(4) 1 d DG U P A 1
F12 F 0.0171(6) -0.43680(12) 0.8317(3) 0.149(3) Uani 0.573(4) 1 d DG U P A 1
F7 F 0.1209(6) -0.57008(12) 0.8240(3) 0.175(4) Uani 0.573(4) 1 d DG U P A 1
F11A F -0.0659(9) -0.4972(6) 0.8330(7) 0.179(4) Uani 0.427(4) 1 d D . P A 2
F10A F 0.0282(16) -0.5147(8) 0.7537(5) 0.192(4) Uani 0.427(4) 1 d D . P A 2
F9A F 0.1996(9) -0.5176(6) 0.8198(8) 0.167(3) Uani 0.427(4) 1 d D . P A 2
F8A F 0.0932(15) -0.4916(7) 0.9027(5) 0.180(4) Uani 0.427(4) 1 d D . P A 2
F12A F 0.0883(13) -0.4405(4) 0.8038(6) 0.149(3) Uani 0.427(4) 1 d D . P A 2
F7A F 0.0576(15) -0.5669(4) 0.8495(8) 0.175(4) Uani 0.427(4) 1 d D . P A 2
Cl1 Cl 0.0034(3) -0.09527(17) 0.25257(16) 0.2120(12) Uani 1 1 d . . . . .
Cl2 Cl -0.1033(7) -0.1765(4) 0.3372(4) 0.2120(12) Uani 0.530(5) 1 d D . P B 1
C43 C -0.1057(12) -0.0991(6) 0.3044(6) 0.2120(12) Uani 1 1 d D . . . .
H43A H -0.183524 -0.090023 0.280195 0.254 Uiso 0.530(5) 1 calc R U P B 1
H43B H -0.089221 -0.071696 0.340946 0.254 Uiso 0.530(5) 1 calc R U P B 1
H43C H -0.122872 -0.060155 0.319205 0.254 Uiso 0.470(5) 1 calc R U P B 2
H43D H -0.178528 -0.114406 0.279763 0.254 Uiso 0.470(5) 1 calc R U P B 2
Cl2A Cl -0.0670(8) -0.1401(4) 0.3697(4) 0.2120(12) Uani 0.470(5) 1 d D . P B 2
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Ni Ni 0.3393 1.1124 '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'
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
C33 Ni1 C38 94.69(18) . . ?
C33 Ni1 P5 169.79(14) . . ?
C38 Ni1 P5 95.19(13) . . ?
C33 Ni1 P3 92.74(14) . . ?
C38 Ni1 P3 117.43(13) . . ?
P5 Ni1 P3 84.98(4) . . ?
C33 Ni1 P4 89.49(14) . . ?
C38 Ni1 P4 110.17(13) . . ?
P5 Ni1 P4 84.70(4) . . ?
P3 Ni1 P4 131.95(5) . . ?
O2 P5 O1 106.67(18) . . ?
O2 P5 C14 101.85(16) . . ?
O1 P5 C14 102.38(16) . . ?
O2 P5 Ni1 112.01(11) . . ?
O1 P5 Ni1 112.12(11) . . ?
C14 P5 Ni1 120.44(13) . . ?
C1 P4 C7 105.52(15) . . ?
C1 P4 C13 104.35(19) . . ?
C7 P4 C13 108.66(19) . . ?
C1 P4 Ni1 118.20(13) . . ?
C7 P4 Ni1 114.45(11) . . ?
C13 P4 Ni1 104.94(15) . . ?
C27 P3 C21 104.87(15) . . ?
C27 P3 C20 105.74(19) . . ?
C21 P3 C20 105.0(2) . . ?
C27 P3 Ni1 116.98(12) . . ?
C21 P3 Ni1 118.13(12) . . ?
C20 P3 Ni1 104.88(15) . . ?
C13 O1 P5 120.8(3) . . ?
C20 O2 P5 119.6(3) . . ?
C38 N2 C39 178.4(5) . . ?
C33 N1 C34 174.7(5) . . ?
N2 C38 Ni1 176.6(4) . . ?
N1 C34 C37 107.0(4) . . ?
N1 C34 C36 106.6(4) . . ?
C37 C34 C36 113.1(6) . . ?
N1 C34 C35 107.5(5) . . ?
C37 C34 C35 110.5(5) . . ?
C36 C34 C35 111.8(6) . . ?
N1 C33 Ni1 176.3(4) . . ?
O1 C13 P4 107.9(3) . . ?
O1 C13 H13A 110.1 . . ?
P4 C13 H13A 110.1 . . ?
O1 C13 H13B 110.1 . . ?
P4 C13 H13B 110.1 . . ?
H13A C13 H13B 108.4 . . ?
C22 C23 C24 120.0 . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C21 C22 C23 120.0 . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C22 C21 C26 120.0 . . ?
C22 C21 P3 119.15(19) . . ?
C26 C21 P3 120.78(19) . . ?
C25 C26 C21 120.0 . . ?
C25 C26 H26 120.0 . . ?
C21 C26 H26 120.0 . . ?
C24 C25 C26 120.0 . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C25 C24 C23 120.0 . . ?
C25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
N2 C39 C41 106.8(4) . . ?
N2 C39 C40 105.3(5) . . ?
C41 C39 C40 112.5(6) . . ?
N2 C39 C42 106.0(5) . . ?
C41 C39 C42 111.3(5) . . ?
C40 C39 C42 114.3(6) . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O2 C20 P3 107.3(3) . . ?
O2 C20 H20A 110.3 . . ?
P3 C20 H20A 110.3 . . ?
O2 C20 H20B 110.3 . . ?
P3 C20 H20B 110.3 . . ?
H20A C20 H20B 108.5 . . ?
C11 C10 C9 120.0 . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C12 C11 C10 120.0 . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C7 C12 C11 120.0 . . ?
C7 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C7 C8 120.0 . . ?
C12 C7 P4 122.69(17) . . ?
C8 C7 P4 117.05(17) . . ?
C7 C8 C9 120.0 . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C8 C9 C10 120.0 . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C1 120.0 . . ?
C5 C6 H6 120.0 . . ?
C1 C6 H6 120.0 . . ?
C2 C1 C6 120.0 . . ?
C2 C1 P4 118.32(19) . . ?
C6 C1 P4 121.61(19) . . ?
C1 C2 C3 120.0 . . ?
C1 C2 H2 120.0 . . ?
C3 C2 H2 120.0 . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C18 C17 C16 120.0 . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C19 C18 C17 120.0 . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C18 C19 C14 120.0 . . ?
C18 C19 H19 120.0 . . ?
C14 C19 H19 120.0 . . ?
C15 C14 C19 120.0 . . ?
C15 C14 P5 120.6(2) . . ?
C19 C14 P5 119.3(2) . . ?
C14 C15 C16 120.0 . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C15 C16 C17 120.0 . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C31 C30 C29 120.0 . . ?
C31 C30 H30 120.0 . . ?
C29 C30 H30 120.0 . . ?
C30 C31 C32 120.0 . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C31 C32 C27 120.0 . . ?
C31 C32 H32 120.0 . . ?
C27 C32 H32 120.0 . . ?
C32 C27 C28 120.0 . . ?
C32 C27 P3 120.45(19) . . ?
C28 C27 P3 119.30(19) . . ?
C29 C28 C27 120.0 . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C28 C29 C30 120.0 . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
F2 P1 F1 91.9(4) . . ?
F2 P1 F5 179.2(3) . . ?
F1 P1 F5 88.2(3) . . ?
F2 P1 F3 91.0(3) . . ?
F1 P1 F3 90.9(3) . . ?
F5 P1 F3 89.8(3) . . ?
F2 P1 F4 91.2(4) . . ?
F1 P1 F4 176.9(3) . . ?
F5 P1 F4 88.7(3) . . ?
F3 P1 F4 88.6(2) . . ?
F2 P1 F6 88.2(2) . . ?
F1 P1 F6 90.4(2) . . ?
F5 P1 F6 91.0(2) . . ?
F3 P1 F6 178.5(2) . . ?
F4 P1 F6 90.1(2) . . ?
F8A P2 F9A 95.1(8) . . ?
F8A P2 F7A 84.1(8) . . ?
F9A P2 F7A 86.9(8) . . ?
F8A P2 F10A 172.8(9) . . ?
F9A P2 F10A 92.0(8) . . ?
F7A P2 F10A 95.5(9) . . ?
F8A P2 F11A 88.3(8) . . ?
F9A P2 F11A 172.8(7) . . ?
F7A P2 F11A 87.2(8) . . ?
F10A P2 F11A 84.5(8) . . ?
F8A P2 F12A 97.4(7) . . ?
F9A P2 F12A 89.5(7) . . ?
F7A P2 F12A 176.2(8) . . ?
F10A P2 F12A 83.5(8) . . ?
F11A P2 F12A 96.3(7) . . ?
F7 P2 F10 90.0 . . ?
F7 P2 F8 90.1 . . ?
F10 P2 F8 179.8 . . ?
F7 P2 F9 90.1 . . ?
F10 P2 F9 90.0 . . ?
F8 P2 F9 90.1 . . ?
F7 P2 F12 180.0 . . ?
F10 P2 F12 90.0 . . ?
F8 P2 F12 89.9 . . ?
F9 P2 F12 89.9 . . ?
F7 P2 F11 90.0 . . ?
F10 P2 F11 90.0 . . ?
F8 P2 F11 89.9 . . ?
F9 P2 F11 179.9 . . ?
F12 P2 F11 90.0 . . ?
Cl2A C43 Cl1 112.6(8) . . ?
Cl1 C43 Cl2 106.3(7) . . ?
Cl1 C43 H43A 110.5 . . ?
Cl2 C43 H43A 110.5 . . ?
Cl1 C43 H43B 110.5 . . ?
Cl2 C43 H43B 110.5 . . ?
H43A C43 H43B 108.7 . . ?
Cl2A C43 H43C 109.1 . . ?
Cl1 C43 H43C 109.1 . . ?
Cl2A C43 H43D 109.1 . . ?
Cl1 C43 H43D 109.1 . . ?
H43C C43 H43D 107.8 . . ?
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 C33 1.866(4) . ?
Ni1 C38 1.955(5) . ?
Ni1 P5 2.1518(11) . ?
Ni1 P3 2.2234(12) . ?
Ni1 P4 2.2255(12) . ?
P5 O2 1.590(3) . ?
P5 O1 1.593(3) . ?
P5 C14 1.772(3) . ?
P4 C1 1.808(2) . ?
P4 C7 1.815(2) . ?
P4 C13 1.851(4) . ?
P3 C27 1.806(2) . ?
P3 C21 1.824(3) . ?
P3 C20 1.857(4) . ?
O1 C13 1.439(5) . ?
O2 C20 1.431(5) . ?
N2 C38 1.139(5) . ?
N2 C39 1.482(6) . ?
N1 C33 1.146(5) . ?
N1 C34 1.475(6) . ?
C34 C37 1.506(8) . ?
C34 C36 1.521(8) . ?
C34 C35 1.531(9) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C23 C22 1.3900 . ?
C23 C24 1.3900 . ?
C23 H23 0.9300 . ?
C22 C21 1.3900 . ?
C22 H22 0.9300 . ?
C21 C26 1.3900 . ?
C26 C25 1.3900 . ?
C26 H26 0.9300 . ?
C25 C24 1.3900 . ?
C25 H25 0.9300 . ?
C24 H24 0.9300 . ?
C39 C41 1.496(7) . ?
C39 C40 1.509(9) . ?
C39 C42 1.513(9) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C10 C11 1.3900 . ?
C10 C9 1.3900 . ?
C10 H10 0.9300 . ?
C11 C12 1.3900 . ?
C11 H11 0.9300 . ?
C12 C7 1.3900 . ?
C12 H12 0.9300 . ?
C7 C8 1.3900 . ?
C8 C9 1.3900 . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C4 C5 1.3900 . ?
C4 C3 1.3900 . ?
C4 H4 0.9300 . ?
C5 C6 1.3900 . ?
C5 H5 0.9300 . ?
C6 C1 1.3900 . ?
C6 H6 0.9300 . ?
C1 C2 1.3900 . ?
C2 C3 1.3900 . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C17 C18 1.3900 . ?
C17 C16 1.3900 . ?
C17 H17 0.9300 . ?
C18 C19 1.3900 . ?
C18 H18 0.9300 . ?
C19 C14 1.3900 . ?
C19 H19 0.9300 . ?
C14 C15 1.3900 . ?
C15 C16 1.3900 . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C30 C31 1.3900 . ?
C30 C29 1.3900 . ?
C30 H30 0.9300 . ?
C31 C32 1.3900 . ?
C31 H31 0.9300 . ?
C32 C27 1.3900 . ?
C32 H32 0.9300 . ?
C27 C28 1.3900 . ?
C28 C29 1.3900 . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
P1 F2 1.543(4) . ?
P1 F1 1.564(4) . ?
P1 F5 1.566(4) . ?
P1 F3 1.571(4) . ?
P1 F4 1.579(4) . ?
P1 F6 1.583(4) . ?
P2 F8A 1.528(11) . ?
P2 F9A 1.529(10) . ?
P2 F7A 1.531(10) . ?
P2 F10A 1.534(11) . ?
P2 F11A 1.540(11) . ?
P2 F12A 1.552(9) . ?
P2 F7 1.6426 . ?
P2 F10 1.6443 . ?
P2 F8 1.6449 . ?
P2 F9 1.6452 . ?
P2 F12 1.6464 . ?
P2 F11 1.6471 . ?
Cl1 C43 1.710(12) . ?
Cl2 C43 1.898(15) . ?
C43 Cl2A 1.637(14) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C43 H43C 0.9700 . ?
C43 H43D 0.9700 . ?
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
O2 P5 O1 C13 113.5(3) . . . . ?
C14 P5 O1 C13 -140.0(3) . . . . ?
Ni1 P5 O1 C13 -9.5(4) . . . . ?
O1 P5 O2 C20 -102.2(4) . . . . ?
C14 P5 O2 C20 150.9(3) . . . . ?
Ni1 P5 O2 C20 20.8(4) . . . . ?
P5 O1 C13 P4 28.0(4) . . . . ?
C1 P4 C13 O1 -157.4(3) . . . . ?
C7 P4 C13 O1 90.4(3) . . . . ?
Ni1 P4 C13 O1 -32.4(3) . . . . ?
C24 C23 C22 C21 0.0 . . . . ?
C23 C22 C21 C26 0.0 . . . . ?
C23 C22 C21 P3 -177.2(2) . . . . ?
C27 P3 C21 C22 49.5(2) . . . . ?
C20 P3 C21 C22 -61.7(2) . . . . ?
Ni1 P3 C21 C22 -178.09(15) . . . . ?
C27 P3 C21 C26 -127.6(2) . . . . ?
C20 P3 C21 C26 121.2(2) . . . . ?
Ni1 P3 C21 C26 4.8(2) . . . . ?
C22 C21 C26 C25 0.0 . . . . ?
P3 C21 C26 C25 177.1(2) . . . . ?
C21 C26 C25 C24 0.0 . . . . ?
C26 C25 C24 C23 0.0 . . . . ?
C22 C23 C24 C25 0.0 . . . . ?
P5 O2 C20 P3 -35.8(5) . . . . ?
C27 P3 C20 O2 157.7(3) . . . . ?
C21 P3 C20 O2 -91.7(3) . . . . ?
Ni1 P3 C20 O2 33.4(4) . . . . ?
C9 C10 C11 C12 0.0 . . . . ?
C10 C11 C12 C7 0.0 . . . . ?
C11 C12 C7 C8 0.0 . . . . ?
C11 C12 C7 P4 174.0(2) . . . . ?
C1 P4 C7 C12 -91.7(2) . . . . ?
C13 P4 C7 C12 19.8(2) . . . . ?
Ni1 P4 C7 C12 136.66(16) . . . . ?
C1 P4 C7 C8 82.5(2) . . . . ?
C13 P4 C7 C8 -166.1(2) . . . . ?
Ni1 P4 C7 C8 -49.21(19) . . . . ?
C12 C7 C8 C9 0.0 . . . . ?
P4 C7 C8 C9 -174.3(2) . . . . ?
C7 C8 C9 C10 0.0 . . . . ?
C11 C10 C9 C8 0.0 . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C4 C5 C6 C1 0.0 . . . . ?
C5 C6 C1 C2 0.0 . . . . ?
C5 C6 C1 P4 -176.9(3) . . . . ?
C7 P4 C1 C2 -169.3(2) . . . . ?
C13 P4 C1 C2 76.3(3) . . . . ?
Ni1 P4 C1 C2 -39.8(2) . . . . ?
C7 P4 C1 C6 7.6(3) . . . . ?
C13 P4 C1 C6 -106.8(3) . . . . ?
Ni1 P4 C1 C6 137.16(19) . . . . ?
C6 C1 C2 C3 0.0 . . . . ?
P4 C1 C2 C3 177.0(3) . . . . ?
C1 C2 C3 C4 0.0 . . . . ?
C5 C4 C3 C2 0.0 . . . . ?
C16 C17 C18 C19 0.0 . . . . ?
C17 C18 C19 C14 0.0 . . . . ?
C18 C19 C14 C15 0.0 . . . . ?
C18 C19 C14 P5 -179.0(3) . . . . ?
O2 P5 C14 C15 139.2(2) . . . . ?
O1 P5 C14 C15 28.9(3) . . . . ?
Ni1 P5 C14 C15 -96.2(2) . . . . ?
O2 P5 C14 C19 -41.8(3) . . . . ?
O1 P5 C14 C19 -152.0(2) . . . . ?
Ni1 P5 C14 C19 82.8(2) . . . . ?
C19 C14 C15 C16 0.0 . . . . ?
P5 C14 C15 C16 179.0(3) . . . . ?
C14 C15 C16 C17 0.0 . . . . ?
C18 C17 C16 C15 0.0 . . . . ?
C29 C30 C31 C32 0.0 . . . . ?
C30 C31 C32 C27 0.0 . . . . ?
C31 C32 C27 C28 0.0 . . . . ?
C31 C32 C27 P3 -174.2(3) . . . . ?
C21 P3 C27 C32 -145.0(2) . . . . ?
C20 P3 C27 C32 -34.3(3) . . . . ?
Ni1 P3 C27 C32 82.0(2) . . . . ?
C21 P3 C27 C28 40.8(3) . . . . ?
C20 P3 C27 C28 151.4(3) . . . . ?
Ni1 P3 C27 C28 -92.3(2) . . . . ?
C32 C27 C28 C29 0.0 . . . . ?
P3 C27 C28 C29 174.3(3) . . . . ?
C27 C28 C29 C30 0.0 . . . . ?
C31 C30 C29 C28 0.0 . . . . ?
