#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:27:18 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179664 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/17/4511784.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_4511784
loop_
_publ_author_name
'Weiss, Charles J.'
'Das, Parthapratim'
'Miller, Deanna L.'
'Helm, Monte L.'
'Appel, Aaron M.'
_publ_section_title
;
 Catalytic Oxidation of Alcohol via Nickel Phosphine Complexes with
 Pendant Amines
;
_journal_issue                   9
_journal_name_full               'ACS Catalysis'
_journal_page_first              2951
_journal_paper_doi               10.1021/cs500853f
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety         '3(C48 H72 N4 Ni P4), 3(B F4), 2(C2 H3 N)'
_chemical_formula_sum            'C148 H222 B3 F12 N14 Ni3 P12'
_chemical_formula_weight         3005.58
_chemical_name_systematic        '[HNi(PtBu2NPh2)](BF4)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-04-15
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2839 for OlexSys, GUI svn.r4713)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.880(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.8297(8)
_cell_length_b                   11.6379(6)
_cell_length_c                   43.244(2)
_cell_measurement_reflns_used    9846
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.85
_cell_measurement_theta_min      2.25
_cell_volume                     7453.9(7)
_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    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            94659
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.938
_diffrn_reflns_theta_min         0.943
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.574
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9119
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0648 before and 0.0568 after correction.
The Ratio of minimum to maximum transmission is 0.9119.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       plate
_exptl_crystal_F_000             3190
_exptl_crystal_recrystallization_method
;
grown by slow diffiusion of XXX into a saturatued solution of the complex in XX
;
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.002
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         17701
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0356P)²+3.4839P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0903
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12952
_reflns_number_total             17701
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cs500853f_si_004.cif
_cod_data_source_block           helm188_0m
_cod_depositor_comments
'Adding full bibliography for 4511782--4511784.cif.'
_cod_original_cell_volume        7454.0(7)
_cod_database_code               4511784
#BEGIN Tags that were not found in dictionaries:
_shelxl_version_number           2013-2
_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_max   0.999
_shelx_estimated_absorpt_t_min   0.894
_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. Others
 Sof(F3A)=1-FVAR(1)
 Sof(F3)=FVAR(1)
 Sof(F2A)=1-FVAR(2)
 Sof(F2)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C25(H25A,H25B), C26(H26A,
 H26B), C27(H27A,H27B), C28(H28A,H28B), C49(H49A,H49B), C50(H50A,H50B),
 C51(H51A,H51B), C52(H52A,H52B)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C20(H20), C21(H21),
 C22(H22), C23(H23), C24(H24), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
  C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C58(H58), C59(H59),
 C60(H60), C61(H61), C62(H62), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C),
 C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C74(H74A,H74B,
 H74C)
;
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, 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 0.24269(2) 0.93379(2) 0.41371(2) 0.01063(6) Uani 1 1 d . . . . .
P1 P 0.11120(3) 1.01466(4) 0.42419(2) 0.01124(11) Uani 1 1 d . . . . .
P2 P 0.16545(3) 0.87666(4) 0.37102(2) 0.01048(11) Uani 1 1 d . . . . .
P3 P 0.37761(3) 1.01745(5) 0.40970(2) 0.01116(11) Uani 1 1 d . . . . .
P4 P 0.31561(3) 0.82970(5) 0.45073(2) 0.01212(11) Uani 1 1 d . . . . .
N1 N 0.11880(11) 1.10606(14) 0.36388(4) 0.0138(4) Uani 1 1 d . . . . .
N2 N 0.04437(10) 0.79611(14) 0.41478(4) 0.0126(4) Uani 1 1 d . . . . .
N3 N 0.36577(11) 1.04374(15) 0.47428(4) 0.0152(4) Uani 1 1 d . . . . .
N4 N 0.44004(11) 0.79717(14) 0.40390(4) 0.0140(4) Uani 1 1 d . . . . .
C1 C 0.06294(14) 1.1006(2) 0.39075(5) 0.0215(5) Uani 1 1 d . . . . .
H1A H 0.0036 1.0675 0.3841 0.026 Uiso 1 1 calc R . . . .
H1B H 0.0522 1.1800 0.3980 0.026 Uiso 1 1 calc R . . . .
C2 C 0.12123(13) 0.99774(17) 0.34703(5) 0.0152(4) Uani 1 1 d . . . . .
H2A H 0.1595 1.0073 0.3291 0.018 Uiso 1 1 calc R . . . .
H2B H 0.0594 0.9788 0.3389 0.018 Uiso 1 1 calc R . . . .
C3 C 0.02124(12) 0.90605(17) 0.42882(5) 0.0139(4) Uani 1 1 d . . . . .
H3A H 0.0122 0.8945 0.4511 0.017 Uiso 1 1 calc R . . . .
H3B H -0.0362 0.9347 0.4190 0.017 Uiso 1 1 calc R . . . .
C4 C 0.05786(12) 0.80472(18) 0.38148(4) 0.0125(4) Uani 1 1 d . . . . .
H4A H 0.0064 0.8477 0.3716 0.015 Uiso 1 1 calc R . . . .
H4B H 0.0567 0.7263 0.3726 0.015 Uiso 1 1 calc R . . . .
C5 C 0.09494(13) 1.11621(17) 0.45709(5) 0.0143(4) Uani 1 1 d . . . . .
C6 C 0.15918(14) 1.21800(19) 0.45352(5) 0.0231(5) Uani 1 1 d . . . . .
H6A H 0.2214 1.1898 0.4530 0.035 Uiso 1 1 calc GR . . . .
H6B H 0.1542 1.2706 0.4711 0.035 Uiso 1 1 calc GR . . . .
H6C H 0.1430 1.2587 0.4342 0.035 Uiso 1 1 calc GR . . . .
C7 C 0.12244(14) 1.05348(19) 0.48710(5) 0.0189(5) Uani 1 1 d . . . . .
H7A H 0.0824 0.9876 0.4897 0.028 Uiso 1 1 calc GR . . . .
H7B H 0.1177 1.1060 0.5046 0.028 Uiso 1 1 calc GR . . . .
H7C H 0.1849 1.0266 0.4862 0.028 Uiso 1 1 calc GR . . . .
C8 C -0.00287(13) 1.15941(18) 0.45830(5) 0.0179(5) Uani 1 1 d . . . . .
H8A H -0.0191 1.2028 0.4394 0.027 Uiso 1 1 calc GR . . . .
H8B H -0.0081 1.2093 0.4764 0.027 Uiso 1 1 calc GR . . . .
H8C H -0.0437 1.0936 0.4599 0.027 Uiso 1 1 calc GR . . . .
C9 C 0.11723(12) 1.20839(18) 0.34618(5) 0.0130(4) Uani 1 1 d . . . . .
C10 C 0.07739(13) 1.31032(18) 0.35597(5) 0.0174(5) Uani 1 1 d . . . . .
H10 H 0.0458 1.3105 0.3745 0.021 Uiso 1 1 calc R . . . .
C11 C 0.08315(14) 1.41099(18) 0.33907(5) 0.0207(5) Uani 1 1 d . . . . .
H11 H 0.0561 1.4790 0.3464 0.025 Uiso 1 1 calc R . . . .
C12 C 0.12751(13) 1.41446(18) 0.31170(5) 0.0188(5) Uani 1 1 d . . . . .
H12 H 0.1315 1.4839 0.3003 0.023 Uiso 1 1 calc R . . . .
C13 C 0.16586(13) 1.31428(19) 0.30141(5) 0.0184(5) Uani 1 1 d . . . . .
H13 H 0.1962 1.3148 0.2826 0.022 Uiso 1 1 calc R . . . .
C14 C 0.16085(13) 1.21306(19) 0.31803(5) 0.0159(4) Uani 1 1 d . . . . .
H14 H 0.1874 1.1453 0.3103 0.019 Uiso 1 1 calc R . . . .
C15 C 0.20871(13) 0.77734(18) 0.34108(5) 0.0146(4) Uani 1 1 d . . . . .
C16 C 0.29665(13) 0.8290(2) 0.32971(5) 0.0218(5) Uani 1 1 d . . . . .
H16A H 0.2832 0.9012 0.3188 0.033 Uiso 1 1 calc GR . . . .
H16B H 0.3242 0.7748 0.3156 0.033 Uiso 1 1 calc GR . . . .
H16C H 0.3386 0.8438 0.3475 0.033 Uiso 1 1 calc GR . . . .
C17 C 0.14086(14) 0.75884(19) 0.31350(5) 0.0186(5) Uani 1 1 d . . . . .
H17A H 0.0842 0.7287 0.3210 0.028 Uiso 1 1 calc GR . . . .
H17B H 0.1658 0.7038 0.2990 0.028 Uiso 1 1 calc GR . . . .
H17C H 0.1293 0.8322 0.3029 0.028 Uiso 1 1 calc GR . . . .
C18 C 0.23070(14) 0.66379(18) 0.35736(5) 0.0206(5) Uani 1 1 d . . . . .
H18A H 0.2688 0.6784 0.3761 0.031 Uiso 1 1 calc GR . . . .
H18B H 0.2629 0.6135 0.3435 0.031 Uiso 1 1 calc GR . . . .
H18C H 0.1746 0.6265 0.3630 0.031 Uiso 1 1 calc GR . . . .
C19 C -0.00569(13) 0.69928(18) 0.42426(5) 0.0144(4) Uani 1 1 d . . . . .
C20 C 0.02014(14) 0.58893(18) 0.41549(5) 0.0194(5) Uani 1 1 d . . . . .
H20 H 0.0698 0.5800 0.4026 0.023 Uiso 1 1 calc R . . . .
C21 C -0.02505(15) 0.4928(2) 0.42513(5) 0.0253(5) Uani 1 1 d . . . . .
H21 H -0.0069 0.4189 0.4185 0.030 Uiso 1 1 calc R . . . .
C22 C -0.09680(15) 0.5028(2) 0.44439(6) 0.0275(5) Uani 1 1 d . . . . .
H22 H -0.1273 0.4364 0.4512 0.033 Uiso 1 1 calc R . . . .
C23 C -0.12277(14) 0.6109(2) 0.45337(5) 0.0236(5) Uani 1 1 d . . . . .
H23 H -0.1717 0.6189 0.4666 0.028 Uiso 1 1 calc R . . . .
C24 C -0.07859(13) 0.70846(19) 0.44342(5) 0.0179(5) Uani 1 1 d . . . . .
H24 H -0.0981 0.7822 0.4497 0.021 Uiso 1 1 calc R . . . .
C25 C 0.42638(13) 1.06108(19) 0.44886(4) 0.0153(4) Uani 1 1 d . . . . .
H25A H 0.4824 1.0167 0.4534 0.018 Uiso 1 1 calc R . . . .
H25B H 0.4431 1.1434 0.4482 0.018 Uiso 1 1 calc R . . . .
C26 C 0.35756(13) 0.92279(18) 0.48305(5) 0.0156(4) Uani 1 1 d . . . . .
H26A H 0.3159 0.9168 0.5001 0.019 Uiso 1 1 calc R . . . .
H26B H 0.4174 0.8944 0.4909 0.019 Uiso 1 1 calc R . . . .
C27 C 0.42375(12) 0.77044(18) 0.43624(4) 0.0136(4) Uani 1 1 d . . . . .
H27A H 0.4748 0.8007 0.4495 0.016 Uiso 1 1 calc R . . . .
H27B H 0.4233 0.6859 0.4387 0.016 Uiso 1 1 calc R . . . .
C28 C 0.46576(13) 0.91557(17) 0.39806(5) 0.0137(4) Uani 1 1 d . . . . .
H28A H 0.4756 0.9254 0.3757 0.016 Uiso 1 1 calc R . . . .
H28B H 0.5232 0.9330 0.4098 0.016 Uiso 1 1 calc R . . . .
C29 C 0.39938(13) 1.14641(17) 0.38523(5) 0.0142(4) Uani 1 1 d . . . . .
C30 C 0.33841(14) 1.24369(18) 0.39589(5) 0.0193(5) Uani 1 1 d . . . . .
H30A H 0.2755 1.2177 0.3949 0.029 Uiso 1 1 calc GR . . . .
H30B H 0.3445 1.3105 0.3824 0.029 Uiso 1 1 calc GR . . . .
H30C H 0.3564 1.2650 0.4172 0.029 Uiso 1 1 calc GR . . . .
C31 C 0.49902(13) 1.18268(19) 0.38729(5) 0.0183(5) Uani 1 1 d . . . . .
H31A H 0.5175 1.1997 0.4089 0.027 Uiso 1 1 calc GR . . . .
H31B H 0.5069 1.2514 0.3746 0.027 Uiso 1 1 calc GR . . . .
H31C H 0.5363 1.1201 0.3797 0.027 Uiso 1 1 calc GR . . . .
C32 C 0.37073(13) 1.11713(19) 0.35159(5) 0.0169(4) Uani 1 1 d . . . . .
H32A H 0.4091 1.0554 0.3442 0.025 Uiso 1 1 calc GR . . . .
H32B H 0.3772 1.1854 0.3386 0.025 Uiso 1 1 calc GR . . . .
H32C H 0.3076 1.0919 0.3504 0.025 Uiso 1 1 calc GR . . . .
C33 C 0.36727(13) 1.12634(19) 0.49841(5) 0.0161(4) Uani 1 1 d . . . . .
C34 C 0.34202(13) 1.0969(2) 0.52822(5) 0.0188(5) Uani 1 1 d . . . . .
H34 H 0.3288 1.0191 0.5329 0.023 Uiso 1 1 calc R . . . .
C35 C 0.33626(14) 1.1804(2) 0.55095(5) 0.0245(5) Uani 1 1 d . . . . .
H35 H 0.3177 1.1592 0.5709 0.029 Uiso 1 1 calc R . . . .
C36 C 0.35697(14) 1.2939(2) 0.54514(6) 0.0261(5) Uani 1 1 d . . . . .
H36 H 0.3532 1.3504 0.5609 0.031 Uiso 1 1 calc R . . . .
C37 C 0.38329(14) 1.3235(2) 0.51597(5) 0.0250(5) Uani 1 1 d . . . . .
H37 H 0.3984 1.4010 0.5117 0.030 Uiso 1 1 calc R . . . .
C38 C 0.38793(14) 1.24210(19) 0.49298(5) 0.0213(5) Uani 1 1 d . . . . .
H38 H 0.4055 1.2648 0.4730 0.026 Uiso 1 1 calc R . . . .
C39 C 0.26980(13) 0.70369(18) 0.47200(5) 0.0153(4) Uani 1 1 d . . . . .
C40 C 0.33668(14) 0.65932(19) 0.49747(5) 0.0209(5) Uani 1 1 d . . . . .
H40A H 0.3935 0.6382 0.4883 0.031 Uiso 1 1 calc GR . . . .
H40B H 0.3112 0.5918 0.5074 0.031 Uiso 1 1 calc GR . . . .
H40C H 0.3481 0.7197 0.5130 0.031 Uiso 1 1 calc GR . . . .
C41 C 0.18144(13) 0.7402(2) 0.48646(5) 0.0212(5) Uani 1 1 d . . . . .
H41A H 0.1945 0.7988 0.5023 0.032 Uiso 1 1 calc GR . . . .
H41B H 0.1537 0.6732 0.4959 0.032 Uiso 1 1 calc GR . . . .
H41C H 0.1398 0.7718 0.4703 0.032 Uiso 1 1 calc GR . . . .
C42 C 0.24834(15) 0.60848(19) 0.44828(5) 0.0221(5) Uani 1 1 d . . . . .
H42A H 0.2122 0.6403 0.4307 0.033 Uiso 1 1 calc GR . . . .
H42B H 0.2143 0.5473 0.4580 0.033 Uiso 1 1 calc GR . . . .
H42C H 0.3048 0.5770 0.4410 0.033 Uiso 1 1 calc GR . . . .
C43 C 0.48143(13) 0.71232(18) 0.38592(5) 0.0136(4) Uani 1 1 d . . . . .
C44 C 0.55634(13) 0.73691(19) 0.36865(5) 0.0164(4) Uani 1 1 d . . . . .
H44 H 0.5872 0.8078 0.3717 0.020 Uiso 1 1 calc R . . . .
C45 C 0.58601(14) 0.65882(19) 0.34712(5) 0.0194(5) Uani 1 1 d . . . . .
H45 H 0.6368 0.6770 0.3355 0.023 Uiso 1 1 calc R . . . .
C46 C 0.54236(14) 0.55493(19) 0.34238(5) 0.0209(5) Uani 1 1 d . . . . .
H46 H 0.5600 0.5040 0.3266 0.025 Uiso 1 1 calc R . . . .
C47 C 0.47234(14) 0.52640(19) 0.36107(5) 0.0203(5) Uani 1 1 d . . . . .
H47 H 0.4440 0.4535 0.3588 0.024 Uiso 1 1 calc R . . . .
C48 C 0.44331(13) 0.60280(18) 0.38293(5) 0.0165(4) Uani 1 1 d . . . . .
H48 H 0.3969 0.5806 0.3961 0.020 Uiso 1 1 calc R . . . .
Ni2 Ni 0.2500 0.85471(3) 0.7500 0.00914(8) Uani 1 2 d S T P . .
P5 P 0.11232(3) 0.92907(4) 0.75481(2) 0.00943(11) Uani 1 1 d . . . . .
P6 P 0.18538(3) 0.77640(4) 0.70734(2) 0.00932(11) Uani 1 1 d . . . . .
N5 N 0.13389(11) 0.99840(14) 0.69310(4) 0.0123(3) Uani 1 1 d . . . . .
N6 N 0.05505(10) 0.70573(14) 0.74945(4) 0.0116(3) Uani 1 1 d . . . . .
C49 C 0.06802(12) 0.99292(17) 0.71711(4) 0.0112(4) Uani 1 1 d . . . . .
H49A H 0.0156 0.9469 0.7092 0.013 Uiso 1 1 calc R . . . .
H49B H 0.0461 1.0717 0.7211 0.013 Uiso 1 1 calc R . . . .
C50 C 0.14791(13) 0.88666(16) 0.67857(4) 0.0118(4) Uani 1 1 d . . . . .
H50A H 0.1939 0.8945 0.6629 0.014 Uiso 1 1 calc R . . . .
H50B H 0.0908 0.8613 0.6678 0.014 Uiso 1 1 calc R . . . .
C51 C 0.07515(12) 0.70788(17) 0.71641(4) 0.0106(4) Uani 1 1 d . . . . .
H51A H 0.0259 0.7495 0.7049 0.013 Uiso 1 1 calc R . . . .
H51B H 0.0750 0.6279 0.7086 0.013 Uiso 1 1 calc R . . . .
C52 C 0.02547(12) 0.81752(16) 0.76065(5) 0.0111(4) Uani 1 1 d . . . . .
H52A H 0.0140 0.8119 0.7830 0.013 Uiso 1 1 calc R . . . .
H52B H -0.0317 0.8398 0.7494 0.013 Uiso 1 1 calc R . . . .
C53 C 0.08564(12) 1.04401(17) 0.78316(5) 0.0122(4) Uani 1 1 d . . . . .
C54 C 0.10906(14) 0.99996(18) 0.81598(5) 0.0160(4) Uani 1 1 d . . . . .
H54A H 0.0694 0.9355 0.8206 0.024 Uiso 1 1 calc GR . . . .
H54B H 0.1008 1.0620 0.8309 0.024 Uiso 1 1 calc GR . . . .
H54C H 0.1720 0.9742 0.8174 0.024 Uiso 1 1 calc GR . . . .
C55 C -0.01395(13) 1.08084(18) 0.78089(5) 0.0159(4) Uani 1 1 d . . . . .
H55A H -0.0294 1.1095 0.7600 0.024 Uiso 1 1 calc GR . . . .
H55B H -0.0237 1.1417 0.7960 0.024 Uiso 1 1 calc GR . . . .
H55C H -0.0522 1.0147 0.7852 0.024 Uiso 1 1 calc GR . . . .
C56 C 0.14806(13) 1.14562(17) 0.77683(5) 0.0161(4) Uani 1 1 d . . . . .
H56A H 0.2111 1.1208 0.7794 0.024 Uiso 1 1 calc GR . . . .
H56B H 0.1371 1.2079 0.7914 0.024 Uiso 1 1 calc GR . . . .
H56C H 0.1358 1.1731 0.7556 0.024 Uiso 1 1 calc GR . . . .
C57 C 0.13925(12) 1.09831(17) 0.67470(5) 0.0126(4) Uani 1 1 d . . . . .
C58 C 0.11705(14) 1.20708(18) 0.68608(5) 0.0172(4) Uani 1 1 d . . . . .
H58 H 0.0948 1.2135 0.7062 0.021 Uiso 1 1 calc R . . . .
C59 C 0.12707(14) 1.30542(18) 0.66844(5) 0.0187(5) Uani 1 1 d . . . . .
H59 H 0.1111 1.3779 0.6767 0.022 Uiso 1 1 calc R . . . .
C60 C 0.15992(13) 1.29964(19) 0.63910(5) 0.0194(5) Uani 1 1 d . . . . .
H60 H 0.1671 1.3672 0.6271 0.023 Uiso 1 1 calc R . . . .
C61 C 0.18203(13) 1.19310(19) 0.62770(5) 0.0188(5) Uani 1 1 d . . . . .
H61 H 0.2049 1.1876 0.6076 0.023 Uiso 1 1 calc R . . . .
C62 C 0.17160(12) 1.09402(18) 0.64487(5) 0.0149(4) Uani 1 1 d . . . . .
H62 H 0.1867 1.0219 0.6363 0.018 Uiso 1 1 calc R . . . .
C63 C 0.23622(12) 0.66473(17) 0.68226(5) 0.0125(4) Uani 1 1 d . . . . .
C64 C 0.26020(13) 0.56196(17) 0.70330(5) 0.0153(4) Uani 1 1 d . . . . .
H64A H 0.3026 0.5866 0.7201 0.023 Uiso 1 1 calc GR . . . .
H64B H 0.2881 0.5016 0.6912 0.023 Uiso 1 1 calc GR . . . .
H64C H 0.2052 0.5320 0.7120 0.023 Uiso 1 1 calc GR . . . .
C65 C 0.17279(13) 0.62852(18) 0.65485(5) 0.0164(4) Uani 1 1 d . . . . .
H65A H 0.1161 0.5995 0.6626 0.025 Uiso 1 1 calc GR . . . .
H65B H 0.2016 0.5680 0.6431 0.025 Uiso 1 1 calc GR . . . .
H65C H 0.1602 0.6949 0.6414 0.025 Uiso 1 1 calc GR . . . .
C66 C 0.32380(13) 0.71258(18) 0.66974(5) 0.0167(4) Uani 1 1 d . . . . .
H66A H 0.3099 0.7804 0.6569 0.025 Uiso 1 1 calc GR . . . .
H66B H 0.3520 0.6538 0.6572 0.025 Uiso 1 1 calc GR . . . .
H66C H 0.3654 0.7341 0.6871 0.025 Uiso 1 1 calc GR . . . .
C67 C 0.00160(12) 0.60964(17) 0.75775(5) 0.0122(4) Uani 1 1 d . . . . .
C68 C 0.03020(13) 0.49867(18) 0.75081(5) 0.0153(4) Uani 1 1 d . . . . .
H68 H 0.0863 0.4885 0.7415 0.018 Uiso 1 1 calc R . . . .
C69 C -0.02096(14) 0.40357(18) 0.75715(5) 0.0186(5) Uani 1 1 d . . . . .
H69 H -0.0008 0.3292 0.7516 0.022 Uiso 1 1 calc R . . . .
C70 C -0.10200(14) 0.41590(19) 0.77159(5) 0.0232(5) Uani 1 1 d . . . . .
H70 H -0.1380 0.3506 0.7757 0.028 Uiso 1 1 calc R . . . .
C71 C -0.12944(14) 0.52457(19) 0.77994(5) 0.0221(5) Uani 1 1 d . . . . .
H71 H -0.1837 0.5333 0.7905 0.027 Uiso 1 1 calc R . . . .
C72 C -0.07909(13) 0.62124(18) 0.77319(5) 0.0158(4) Uani 1 1 d . . . . .
H72 H -0.0992 0.6953 0.7790 0.019 Uiso 1 1 calc R . . . .
F1 F 0.18785(8) 0.98350(12) 0.57060(3) 0.0339(3) Uani 1 1 d . . . . .
F2 F 0.1926(7) 0.8337(5) 0.60102(14) 0.059(2) Uani 0.71(3) 1 d . . P A 1
F3 F 0.3117(4) 0.9624(13) 0.60145(13) 0.044(2) Uani 0.62(3) 1 d . . P A 1
F4 F 0.28444(13) 0.84006(14) 0.55984(4) 0.0579(5) Uani 1 1 d . . . . .
B1 B 0.2403(2) 0.8964(3) 0.58284(7) 0.0430(9) Uani 1 1 d . . . . .
N7 N 0.50192(15) 0.56775(19) 0.55379(5) 0.0362(5) Uani 1 1 d . . . . .
C73 C 0.43661(17) 0.5747(2) 0.56648(5) 0.0271(5) Uani 1 1 d . . . . .
C74 C 0.35299(16) 0.5833(2) 0.58293(6) 0.0318(6) Uani 1 1 d . . . . .
H74A H 0.3031 0.5500 0.5702 0.048 Uiso 1 1 calc GR . . . .
H74B H 0.3400 0.6643 0.5871 0.048 Uiso 1 1 calc GR . . . .
H74C H 0.3599 0.5415 0.6026 0.048 Uiso 1 1 calc GR . . . .
F5 F 0.30550(9) 0.12185(13) 0.26911(3) 0.0391(4) Uani 1 1 d . . . . .
F6 F 0.19635(10) -0.01348(13) 0.26816(3) 0.0413(4) Uani 1 1 d . . . . .
B2 B 0.2500 0.0533(3) 0.2500 0.0215(8) Uani 1 2 d S T P . .
F3A F 0.2905(11) 0.900(3) 0.6070(3) 0.060(6) Uani 0.38(3) 1 d . . P A 2
F2A F 0.1717(6) 0.787(2) 0.5898(7) 0.074(7) Uani 0.29(3) 1 d . . P A 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'
B B 0.0013 0.0007 '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'
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
P1 Ni1 P3 128.71(2) . .
P1 Ni1 P4 118.54(2) . .
P2 Ni1 P1 82.87(2) . .
P2 Ni1 P3 119.36(2) . .
P2 Ni1 P4 129.85(2) . .
P3 Ni1 P4 83.65(2) . .
C1 P1 Ni1 111.88(6) . .
C1 P1 C5 100.99(10) . .
C3 P1 Ni1 112.01(6) . .
C3 P1 C1 101.45(10) . .
C3 P1 C5 103.12(9) . .
C5 P1 Ni1 124.53(7) . .
C2 P2 Ni1 113.00(7) . .
C2 P2 C4 101.14(9) . .
C2 P2 C15 101.92(9) . .
C4 P2 Ni1 109.98(6) . .
C15 P2 Ni1 125.32(7) . .
C15 P2 C4 102.48(9) . .
C25 P3 Ni1 110.66(6) . .
C28 P3 Ni1 112.83(7) . .
C28 P3 C25 99.96(9) . .
C28 P3 C29 102.43(9) . .
C29 P3 Ni1 124.88(6) . .
C29 P3 C25 102.90(10) . .
C26 P4 Ni1 110.78(7) . .
C26 P4 C27 101.89(9) . .
C26 P4 C39 101.74(9) . .
C27 P4 Ni1 110.42(6) . .
C39 P4 Ni1 126.79(7) . .
C39 P4 C27 102.26(9) . .
C2 N1 C1 112.91(17) . .
C9 N1 C1 118.14(16) . .
C9 N1 C2 117.23(16) . .
C3 N2 C4 113.19(16) . .
C19 N2 C3 115.88(15) . .
C19 N2 C4 115.87(16) . .
C26 N3 C25 112.83(16) . .
C33 N3 C25 118.05(16) . .
C33 N3 C26 117.34(16) . .
C28 N4 C27 115.09(16) . .
C43 N4 C27 118.23(16) . .
C43 N4 C28 116.13(15) . .
P1 C1 H1A 108.4 . .
P1 C1 H1B 108.4 . .
N1 C1 P1 115.30(14) . .
N1 C1 H1A 108.4 . .
N1 C1 H1B 108.4 . .
H1A C1 H1B 107.5 . .
P2 C2 H2A 108.9 . .
P2 C2 H2B 108.9 . .
N1 C2 P2 113.29(14) . .
N1 C2 H2A 108.9 . .
N1 C2 H2B 108.9 . .
H2A C2 H2B 107.7 . .
P1 C3 H3A 109.3 . .
P1 C3 H3B 109.3 . .
N2 C3 P1 111.44(12) . .
N2 C3 H3A 109.3 . .
N2 C3 H3B 109.3 . .
H3A C3 H3B 108.0 . .
P2 C4 H4A 108.5 . .
P2 C4 H4B 108.5 . .
N2 C4 P2 115.25(13) . .
N2 C4 H4A 108.5 . .
N2 C4 H4B 108.5 . .
H4A C4 H4B 107.5 . .
C6 C5 P1 107.86(14) . .
C6 C5 C8 110.04(17) . .
C7 C5 P1 107.74(14) . .
C7 C5 C6 108.32(17) . .
C7 C5 C8 109.84(16) . .
C8 C5 P1 112.91(14) . .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
H6A C6 H6B 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C5 C7 H7A 109.5 . .
C5 C7 H7B 109.5 . .
C5 C7 H7C 109.5 . .
H7A C7 H7B 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C5 C8 H8A 109.5 . .
C5 C8 H8B 109.5 . .
C5 C8 H8C 109.5 . .
H8A C8 H8B 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C10 C9 N1 123.04(18) . .
C10 C9 C14 116.60(19) . .
C14 C9 N1 120.29(18) . .
C9 C10 H10 119.4 . .
C11 C10 C9 121.26(19) . .
C11 C10 H10 119.4 . .
C10 C11 H11 119.3 . .
C12 C11 C10 121.4(2) . .
C12 C11 H11 119.3 . .
C11 C12 H12 120.9 . .
C13 C12 C11 118.2(2) . .
C13 C12 H12 120.9 . .
C12 C13 H13 119.4 . .
C12 C13 C14 121.2(2) . .
C14 C13 H13 119.4 . .
C9 C14 H14 119.3 . .
C13 C14 C9 121.4(2) . .
C13 C14 H14 119.3 . .
C16 C15 P2 107.76(14) . .
C17 C15 P2 112.93(14) . .
C17 C15 C16 109.82(17) . .
C18 C15 P2 106.76(14) . .
C18 C15 C16 108.72(17) . .
C18 C15 C17 110.71(17) . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16B 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C15 C17 H17A 109.5 . .
C15 C17 H17B 109.5 . .
C15 C17 H17C 109.5 . .
H17A C17 H17B 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C15 C18 H18A 109.5 . .
C15 C18 H18B 109.5 . .
C15 C18 H18C 109.5 . .
H18A C18 H18B 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C20 C19 N2 119.74(17) . .
C20 C19 C24 117.47(19) . .
C24 C19 N2 122.73(18) . .
C19 C20 H20 119.4 . .
C21 C20 C19 121.27(19) . .
C21 C20 H20 119.4 . .
C20 C21 H21 119.6 . .
C20 C21 C22 120.8(2) . .
C22 C21 H21 119.6 . .
C21 C22 H22 120.7 . .
C23 C22 C21 118.6(2) . .
C23 C22 H22 120.7 . .
C22 C23 H23 119.5 . .
C22 C23 C24 121.1(2) . .
C24 C23 H23 119.5 . .
C19 C24 H24 119.6 . .
C23 C24 C19 120.8(2) . .
C23 C24 H24 119.6 . .
P3 C25 H25A 108.6 . .
P3 C25 H25B 108.6 . .
N3 C25 P3 114.55(13) . .
N3 C25 H25A 108.6 . .
N3 C25 H25B 108.6 . .
H25A C25 H25B 107.6 . .
P4 C26 H26A 108.9 . .
P4 C26 H26B 108.9 . .
N3 C26 P4 113.33(14) . .
N3 C26 H26A 108.9 . .
N3 C26 H26B 108.9 . .
H26A C26 H26B 107.7 . .
P4 C27 H27A 108.5 . .
P4 C27 H27B 108.5 . .
N4 C27 P4 115.10(13) . .
N4 C27 H27A 108.5 . .
N4 C27 H27B 108.5 . .
H27A C27 H27B 107.5 . .
P3 C28 H28A 109.4 . .
P3 C28 H28B 109.4 . .
N4 C28 P3 111.35(12) . .
N4 C28 H28A 109.4 . .
N4 C28 H28B 109.4 . .
H28A C28 H28B 108.0 . .
C30 C29 P3 107.49(13) . .
C30 C29 C31 111.08(17) . .
C31 C29 P3 112.35(14) . .
C32 C29 P3 108.09(14) . .
C32 C29 C30 108.04(17) . .
C32 C29 C31 109.65(16) . .
C29 C30 H30A 109.5 . .
C29 C30 H30B 109.5 . .
C29 C30 H30C 109.5 . .
H30A C30 H30B 109.5 . .
H30A C30 H30C 109.5 . .
H30B C30 H30C 109.5 . .
C29 C31 H31A 109.5 . .
C29 C31 H31B 109.5 . .
C29 C31 H31C 109.5 . .
H31A C31 H31B 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
C29 C32 H32A 109.5 . .
C29 C32 H32B 109.5 . .
C29 C32 H32C 109.5 . .
H32A C32 H32B 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
C34 C33 N3 121.0(2) . .
C34 C33 C38 117.3(2) . .
C38 C33 N3 121.51(19) . .
C33 C34 H34 119.7 . .
C35 C34 C33 120.6(2) . .
C35 C34 H34 119.7 . .
C34 C35 H35 119.4 . .
C36 C35 C34 121.2(2) . .
C36 C35 H35 119.4 . .
C35 C36 H36 120.7 . .
C35 C36 C37 118.7(2) . .
C37 C36 H36 120.7 . .
C36 C37 H37 119.5 . .
C38 C37 C36 120.9(2) . .
C38 C37 H37 119.5 . .
C33 C38 H38 119.3 . .
C37 C38 C33 121.3(2) . .
C37 C38 H38 119.3 . .
C40 C39 P4 112.22(14) . .
C40 C39 C41 109.52(17) . .
C41 C39 P4 108.66(14) . .
C42 C39 P4 107.76(14) . .
C42 C39 C40 110.01(17) . .
C42 C39 C41 108.59(17) . .
C39 C40 H40A 109.5 . .
C39 C40 H40B 109.5 . .
C39 C40 H40C 109.5 . .
H40A C40 H40B 109.5 . .
H40A C40 H40C 109.5 . .
H40B C40 H40C 109.5 . .
C39 C41 H41A 109.5 . .
C39 C41 H41B 109.5 . .
C39 C41 H41C 109.5 . .
H41A C41 H41B 109.5 . .
H41A C41 H41C 109.5 . .
H41B C41 H41C 109.5 . .
C39 C42 H42A 109.5 . .
C39 C42 H42B 109.5 . .
C39 C42 H42C 109.5 . .
H42A C42 H42B 109.5 . .
H42A C42 H42C 109.5 . .
H42B C42 H42C 109.5 . .
C44 C43 N4 121.89(18) . .
C48 C43 N4 120.16(17) . .
C48 C43 C44 117.74(19) . .
C43 C44 H44 119.6 . .
C45 C44 C43 120.7(2) . .
C45 C44 H44 119.6 . .
C44 C45 H45 119.7 . .
C46 C45 C44 120.67(19) . .
C46 C45 H45 119.7 . .
C45 C46 H46 120.6 . .
C45 C46 C47 118.8(2) . .
C47 C46 H46 120.6 . .
C46 C47 H47 119.6 . .
C48 C47 C46 120.8(2) . .
C48 C47 H47 119.6 . .
C43 C48 H48 119.6 . .
C47 C48 C43 120.77(19) . .
C47 C48 H48 119.6 . .
P5 Ni2 P5 134.48(3) 2_556 .
P6 Ni2 P5 83.036(18) 2_556 2_556
P6 Ni2 P5 115.939(18) . 2_556
P6 Ni2 P5 83.039(18) . .
P6 Ni2 P5 115.933(18) 2_556 .
P6 Ni2 P6 131.77(3) . 2_556
C49 P5 Ni2 110.67(6) . .
C52 P5 Ni2 112.65(6) . .
C52 P5 C49 100.37(9) . .
C52 P5 C53 103.90(9) . .
C53 P5 Ni2 124.18(6) . .
C53 P5 C49 102.10(9) . .
C50 P6 Ni2 111.98(7) . .
C50 P6 C51 101.51(9) . .
C50 P6 C63 101.97(9) . .
C51 P6 Ni2 110.07(6) . .
C63 P6 Ni2 126.37(7) . .
C63 P6 C51 101.89(9) . .
C49 N5 C50 112.36(15) . .
C57 N5 C49 119.61(15) . .
C57 N5 C50 118.43(15) . .
C52 N6 C51 112.60(15) . .
C67 N6 C51 113.50(15) . .
C67 N6 C52 115.72(15) . .
P5 C49 H49A 108.6 . .
P5 C49 H49B 108.6 . .
N5 C49 P5 114.60(13) . .
N5 C49 H49A 108.6 . .
N5 C49 H49B 108.6 . .
H49A C49 H49B 107.6 . .
P6 C50 H50A 109.3 . .
P6 C50 H50B 109.3 . .
N5 C50 P6 111.80(13) . .
N5 C50 H50A 109.3 . .
N5 C50 H50B 109.3 . .
H50A C50 H50B 107.9 . .
P6 C51 H51A 108.4 . .
P6 C51 H51B 108.4 . .
N6 C51 P6 115.47(13) . .
N6 C51 H51A 108.4 . .
N6 C51 H51B 108.4 . .
H51A C51 H51B 107.5 . .
P5 C52 H52A 109.5 . .
P5 C52 H52B 109.5 . .
N6 C52 P5 110.82(12) . .
N6 C52 H52A 109.5 . .
N6 C52 H52B 109.5 . .
H52A C52 H52B 108.1 . .
C54 C53 P5 108.80(13) . .
C54 C53 C55 108.98(16) . .
C54 C53 C56 108.21(16) . .
C55 C53 P5 113.07(14) . .
C56 C53 P5 106.54(13) . .
C56 C53 C55 111.11(16) . .
C53 C54 H54A 109.5 . .
C53 C54 H54B 109.5 . .
C53 C54 H54C 109.5 . .
H54A C54 H54B 109.5 . .
H54A C54 H54C 109.5 . .
H54B C54 H54C 109.5 . .
C53 C55 H55A 109.5 . .
C53 C55 H55B 109.5 . .
C53 C55 H55C 109.5 . .
H55A C55 H55B 109.5 . .
H55A C55 H55C 109.5 . .
H55B C55 H55C 109.5 . .
C53 C56 H56A 109.5 . .
C53 C56 H56B 109.5 . .
C53 C56 H56C 109.5 . .
H56A C56 H56B 109.5 . .
H56A C56 H56C 109.5 . .
H56B C56 H56C 109.5 . .
C58 C57 N5 121.60(18) . .
C62 C57 N5 121.40(18) . .
C62 C57 C58 116.92(19) . .
C57 C58 H58 119.4 . .
C59 C58 C57 121.19(19) . .
C59 C58 H58 119.4 . .
C58 C59 H59 119.5 . .
C60 C59 C58 121.1(2) . .
C60 C59 H59 119.5 . .
C59 C60 H60 120.9 . .
C61 C60 C59 118.2(2) . .
C61 C60 H60 120.9 . .
C60 C61 H61 119.3 . .
C60 C61 C62 121.5(2) . .
C62 C61 H61 119.3 . .
C57 C62 H62 119.4 . .
C61 C62 C57 121.1(2) . .
C61 C62 H62 119.4 . .
C64 C63 P6 106.58(13) . .
C64 C63 C65 111.03(17) . .
C64 C63 C66 108.47(16) . .
C65 C63 P6 112.85(13) . .
C65 C63 C66 108.88(16) . .
C66 C63 P6 108.92(13) . .
C63 C64 H64A 109.5 . .
C63 C64 H64B 109.5 . .
C63 C64 H64C 109.5 . .
H64A C64 H64B 109.5 . .
H64A C64 H64C 109.5 . .
H64B C64 H64C 109.5 . .
C63 C65 H65A 109.5 . .
C63 C65 H65B 109.5 . .
C63 C65 H65C 109.5 . .
H65A C65 H65B 109.5 . .
H65A C65 H65C 109.5 . .
H65B C65 H65C 109.5 . .
C63 C66 H66A 109.5 . .
C63 C66 H66B 109.5 . .
C63 C66 H66C 109.5 . .
H66A C66 H66B 109.5 . .
H66A C66 H66C 109.5 . .
H66B C66 H66C 109.5 . .
C68 C67 N6 119.48(17) . .
C68 C67 C72 117.76(18) . .
C72 C67 N6 122.76(18) . .
C67 C68 H68 119.2 . .
C69 C68 C67 121.60(18) . .
C69 C68 H68 119.2 . .
C68 C69 H69 119.9 . .
C68 C69 C70 120.3(2) . .
C70 C69 H69 119.9 . .
C69 C70 H70 120.5 . .
C71 C70 C69 118.99(19) . .
C71 C70 H70 120.5 . .
C70 C71 H71 119.4 . .
C70 C71 C72 121.17(19) . .
C72 C71 H71 119.4 . .
C67 C72 H72 120.0 . .
C71 C72 C67 120.1(2) . .
C71 C72 H72 120.0 . .
F1 B1 F3 101.5(5) . .
F1 B1 F4 110.7(2) . .
F1 B1 F2A 107.3(5) . .
F2 B1 F1 109.5(4) . .
F2 B1 F3 110.5(7) . .
F2 B1 F4 117.2(4) . .
F4 B1 F3 106.3(3) . .
F4 B1 F2A 94.7(13) . .
F3A B1 F1 126.8(12) . .
F3A B1 F4 109.5(4) . .
F3A B1 F2A 103(2) . .
N7 C73 C74 179.7(3) . .
C73 C74 H74A 109.5 . .
C73 C74 H74B 109.5 . .
C73 C74 H74C 109.5 . .
H74A C74 H74B 109.5 . .
H74A C74 H74C 109.5 . .
H74B C74 H74C 109.5 . .
F5 B2 F5 109.8(3) 2 .
F6 B2 F5 108.98(9) 2 2
F6 B2 F5 108.65(8) . 2
F6 B2 F5 108.65(8) 2 .
F6 B2 F5 108.99(9) . .
F6 B2 F6 111.7(3) 2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 P1 2.2321(5) .
Ni1 P2 2.2247(6) .
Ni1 P3 2.2397(5) .
Ni1 P4 2.2418(6) .
P1 C1 1.871(2) .
P1 C3 1.856(2) .
P1 C5 1.874(2) .
P2 C2 1.850(2) .
P2 C4 1.8771(19) .
P2 C15 1.873(2) .
P3 C25 1.878(2) .
P3 C28 1.8532(19) .
P3 C29 1.874(2) .
P4 C26 1.851(2) .
P4 C27 1.8818(19) .
P4 C39 1.877(2) .
N1 C1 1.462(2) .
N1 C2 1.457(3) .
N1 C9 1.415(3) .
N2 C3 1.464(2) .
N2 C4 1.467(2) .
N2 C19 1.421(3) .
N3 C25 1.468(2) .
N3 C26 1.464(3) .
N3 C33 1.418(3) .
N4 C27 1.465(2) .
N4 C28 1.455(3) .
N4 C43 1.416(2) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 C6 1.533(3) .
C5 C7 1.527(3) .
C5 C8 1.539(3) .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 C10 1.400(3) .
C9 C14 1.408(3) .
C10 H10 0.9500 .
C10 C11 1.386(3) .
C11 H11 0.9500 .
C11 C12 1.383(3) .
C12 H12 0.9500 .
C12 C13 1.381(3) .
C13 H13 0.9500 .
C13 C14 1.384(3) .
C14 H14 0.9500 .
C15 C16 1.539(3) .
C15 C17 1.537(3) .
C15 C18 1.525(3) .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C19 C20 1.398(3) .
C19 C24 1.399(3) .
C20 H20 0.9500 .
C20 C21 1.379(3) .
C21 H21 0.9500 .
C21 C22 1.389(3) .
C22 H22 0.9500 .
C22 C23 1.377(3) .
C23 H23 0.9500 .
C23 C24 1.390(3) .
C24 H24 0.9500 .
C25 H25A 0.9900 .
C25 H25B 0.9900 .
C26 H26A 0.9900 .
C26 H26B 0.9900 .
C27 H27A 0.9900 .
C27 H27B 0.9900 .
C28 H28A 0.9900 .
C28 H28B 0.9900 .
C29 C30 1.534(3) .
C29 C31 1.535(3) .
C29 C32 1.533(3) .
C30 H30A 0.9800 .
C30 H30B 0.9800 .
C30 H30C 0.9800 .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
C32 H32A 0.9800 .
C32 H32B 0.9800 .
C32 H32C 0.9800 .
C33 C34 1.403(3) .
C33 C38 1.404(3) .
C34 H34 0.9500 .
C34 C35 1.388(3) .
C35 H35 0.9500 .
C35 C36 1.382(3) .
C36 H36 0.9500 .
C36 C37 1.383(3) .
C37 H37 0.9500 .
C37 C38 1.377(3) .
C38 H38 0.9500 .
C39 C40 1.534(3) .
C39 C41 1.540(3) .
C39 C42 1.532(3) .
C40 H40A 0.9800 .
C40 H40B 0.9800 .
C40 H40C 0.9800 .
C41 H41A 0.9800 .
C41 H41B 0.9800 .
C41 H41C 0.9800 .
C42 H42A 0.9800 .
C42 H42B 0.9800 .
C42 H42C 0.9800 .
C43 C44 1.399(3) .
C43 C48 1.398(3) .
C44 H44 0.9500 .
C44 C45 1.389(3) .
C45 H45 0.9500 .
C45 C46 1.382(3) .
C46 H46 0.9500 .
C46 C47 1.388(3) .
C47 H47 0.9500 .
C47 C48 1.382(3) .
C48 H48 0.9500 .
Ni2 P5 2.2369(5) 2_556
Ni2 P5 2.2369(5) .
Ni2 P6 2.2306(5) 2_556
Ni2 P6 2.2305(5) .
P5 C49 1.880(2) .
P5 C52 1.8549(19) .
P5 C53 1.870(2) .
P6 C50 1.853(2) .
P6 C51 1.8778(18) .
P6 C63 1.875(2) .
N5 C49 1.462(2) .
N5 C50 1.464(2) .
N5 C57 1.413(2) .
N6 C51 1.475(2) .
N6 C52 1.463(2) .
N6 C67 1.427(2) .
C49 H49A 0.9900 .
C49 H49B 0.9900 .
C50 H50A 0.9900 .
C50 H50B 0.9900 .
C51 H51A 0.9900 .
C51 H51B 0.9900 .
C52 H52A 0.9900 .
C52 H52B 0.9900 .
C53 C54 1.532(3) .
C53 C55 1.536(3) .
C53 C56 1.535(3) .
C54 H54A 0.9800 .
C54 H54B 0.9800 .
C54 H54C 0.9800 .
C55 H55A 0.9800 .
C55 H55B 0.9800 .
C55 H55C 0.9800 .
C56 H56A 0.9800 .
C56 H56B 0.9800 .
C56 H56C 0.9800 .
C57 C58 1.403(3) .
C57 C62 1.400(3) .
C58 H58 0.9500 .
C58 C59 1.387(3) .
C59 H59 0.9500 .
C59 C60 1.383(3) .
C60 H60 0.9500 .
C60 C61 1.380(3) .
C61 H61 0.9500 .
C61 C62 1.384(3) .
C62 H62 0.9500 .
C63 C64 1.534(3) .
C63 C65 1.535(3) .
C63 C66 1.536(3) .
C64 H64A 0.9800 .
C64 H64B 0.9800 .
C64 H64C 0.9800 .
C65 H65A 0.9800 .
C65 H65B 0.9800 .
C65 H65C 0.9800 .
C66 H66A 0.9800 .
C66 H66B 0.9800 .
C66 H66C 0.9800 .
C67 C68 1.397(3) .
C67 C72 1.406(3) .
C68 H68 0.9500 .
C68 C69 1.377(3) .
C69 H69 0.9500 .
C69 C70 1.389(3) .
C70 H70 0.9500 .
C70 C71 1.382(3) .
C71 H71 0.9500 .
C71 C72 1.389(3) .
C72 H72 0.9500 .
F1 B1 1.367(3) .
F2 B1 1.306(8) .
F3 B1 1.508(11) .
F4 B1 1.384(3) .
B1 F3A 1.255(7) .
B1 F2A 1.668(17) .
N7 C73 1.140(3) .
C73 C74 1.464(3) .
C74 H74A 0.9800 .
C74 H74B 0.9800 .
C74 H74C 0.9800 .
F5 B2 1.389(3) .
F6 B2 1.384(2) .
B2 F5 1.389(3) 2
B2 F6 1.384(2) 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
Ni1 P1 C1 N1 -2.43(19)
Ni1 P1 C3 N2 -19.21(16)
Ni1 P1 C5 C6 57.43(16)
Ni1 P1 C5 C7 -59.30(15)
Ni1 P1 C5 C8 179.23(11)
Ni1 P2 C2 N1 -18.18(16)
Ni1 P2 C4 N2 -1.37(16)
Ni1 P2 C15 C16 -55.76(17)
Ni1 P2 C15 C17 -177.22(11)
Ni1 P2 C15 C18 60.88(15)
Ni1 P3 C25 N3 -5.55(17)
Ni1 P3 C28 N4 -19.47(16)
Ni1 P3 C29 C30 57.82(16)
Ni1 P3 C29 C31 -179.67(11)
Ni1 P3 C29 C32 -58.56(15)
Ni1 P4 C26 N3 -21.01(15)
Ni1 P4 C27 N4 -2.34(17)
Ni1 P4 C39 C40 -175.76(11)
Ni1 P4 C39 C41 -54.51(17)
Ni1 P4 C39 C42 62.98(15)
N1 C9 C10 C11 175.10(19)
N1 C9 C14 C13 -175.30(18)
N2 C19 C20 C21 177.8(2)
N2 C19 C24 C23 -176.76(19)
N3 C33 C34 C35 -174.44(18)
N3 C33 C38 C37 175.50(19)
N4 C43 C44 C45 -168.67(19)
N4 C43 C48 C47 167.68(19)
C1 P1 C3 N2 100.27(15)
C1 P1 C5 C6 -69.05(16)
C1 P1 C5 C7 174.22(14)
C1 P1 C5 C8 52.75(16)
C1 N1 C2 P2 -59.19(19)
C1 N1 C9 C10 11.1(3)
C1 N1 C9 C14 -172.15(19)
C2 P2 C4 N2 -121.06(15)
C2 P2 C15 C16 73.96(16)
C2 P2 C15 C17 -47.50(16)
C2 P2 C15 C18 -169.40(13)
C2 N1 C1 P1 71.8(2)
C2 N1 C9 C10 151.63(19)
C2 N1 C9 C14 -31.7(3)
C3 P1 C1 N1 -122.00(17)
C3 P1 C5 C6 -173.71(14)
C3 P1 C5 C7 69.57(15)
C3 P1 C5 C8 -51.90(16)
C3 N2 C4 P2 73.37(18)
C3 N2 C19 C20 -171.04(18)
C3 N2 C19 C24 6.1(3)
C4 P2 C2 N1 99.34(14)
C4 P2 C15 C16 178.38(14)
C4 P2 C15 C17 56.92(16)
C4 P2 C15 C18 -64.98(15)
C4 N2 C3 P1 -59.78(18)
C4 N2 C19 C20 52.8(2)
C4 N2 C19 C24 -130.1(2)
C5 P1 C1 N1 132.02(17)
C5 P1 C3 N2 -155.43(14)
C9 N1 C1 P1 -146.11(15)
C9 N1 C2 P2 158.32(13)
C9 C10 C11 C12 0.8(3)
C10 C9 C14 C13 1.6(3)
C10 C11 C12 C13 0.4(3)
C11 C12 C13 C14 -0.5(3)
C12 C13 C14 C9 -0.6(3)
C14 C9 C10 C11 -1.7(3)
C15 P2 C2 N1 -155.19(14)
C15 P2 C4 N2 133.92(15)
C19 N2 C3 P1 162.89(14)
C19 N2 C4 P2 -149.29(14)
C19 C20 C21 C22 -1.2(4)
C20 C19 C24 C23 0.4(3)
C20 C21 C22 C23 0.8(4)
C21 C22 C23 C24 0.1(4)
C22 C23 C24 C19 -0.8(3)
C24 C19 C20 C21 0.6(3)
C25 P3 C28 N4 98.08(15)
C25 P3 C29 C30 -69.11(15)
C25 P3 C29 C31 53.40(16)
C25 P3 C29 C32 174.50(13)
C25 N3 C26 P4 -58.41(19)
C25 N3 C33 C34 -154.18(18)
C25 N3 C33 C38 30.3(3)
C26 P4 C27 N4 -120.07(15)
C26 P4 C39 C40 -48.33(16)
C26 P4 C39 C41 72.92(16)
C26 P4 C39 C42 -169.59(14)
C26 N3 C25 P3 74.73(19)
C26 N3 C33 C34 -13.8(3)
C26 N3 C33 C38 170.65(18)
C27 P4 C26 N3 96.46(15)
C27 P4 C39 C40 56.77(16)
C27 P4 C39 C41 178.02(14)
C27 P4 C39 C42 -64.49(15)
C27 N4 C28 P3 -59.33(19)
C27 N4 C43 C44 -129.6(2)
C27 N4 C43 C48 55.8(3)
C28 P3 C25 N3 -124.71(15)
C28 P3 C29 C30 -172.54(14)
C28 P3 C29 C31 -50.03(16)
C28 P3 C29 C32 71.07(14)
C28 N4 C27 P4 73.42(19)
C28 N4 C43 C44 13.5(3)
C28 N4 C43 C48 -161.11(18)
C29 P3 C25 N3 129.96(15)
C29 P3 C28 N4 -156.21(14)
C33 N3 C25 P3 -143.19(15)
C33 N3 C26 P4 159.22(14)
C33 C34 C35 C36 -1.4(3)
C34 C33 C38 C37 -0.2(3)
C34 C35 C36 C37 0.4(3)
C35 C36 C37 C38 0.7(3)
C36 C37 C38 C33 -0.8(3)
C38 C33 C34 C35 1.3(3)
C39 P4 C26 N3 -158.15(14)
C39 P4 C27 N4 134.95(15)
C43 N4 C27 P4 -143.11(15)
C43 N4 C28 P3 156.42(14)
C43 C44 C45 C46 -0.3(3)
C44 C43 C48 C47 -7.1(3)
C44 C45 C46 C47 -4.6(3)
C45 C46 C47 C48 3.5(3)
C46 C47 C48 C43 2.5(3)
C48 C43 C44 C45 6.0(3)
Ni2 P5 C49 N5 -8.40(16)
Ni2 P5 C52 N6 -21.61(15)
Ni2 P5 C53 C54 -60.15(15)
Ni2 P5 C53 C55 178.63(11)
Ni2 P5 C53 C56 56.31(15)
Ni2 P6 C50 N5 -22.98(14)
Ni2 P6 C51 N6 -6.31(16)
Ni2 P6 C63 C64 57.16(15)
Ni2 P6 C63 C65 179.29(11)
Ni2 P6 C63 C66 -59.68(16)
N5 C57 C58 C59 176.55(18)
N5 C57 C62 C61 -175.91(18)
N6 C67 C68 C69 -177.17(19)
N6 C67 C72 C71 178.33(19)
C49 P5 C52 N6 96.11(14)
C49 P5 C53 C54 174.26(13)
C49 P5 C53 C55 53.04(16)
C49 P5 C53 C56 -69.29(14)
C49 N5 C50 P6 -57.63(18)
C49 N5 C57 C58 29.4(3)
C49 N5 C57 C62 -154.11(18)
C50 P6 C51 N6 -125.06(14)
C50 P6 C63 C64 -173.69(13)
C50 P6 C63 C65 -51.57(16)
C50 P6 C63 C66 69.47(15)
C50 N5 C49 P5 77.07(18)
C50 N5 C57 C58 173.00(17)
C50 N5 C57 C62 -10.5(3)
C51 P6 C50 N5 94.39(14)
C51 P6 C63 C64 -69.03(14)
C51 P6 C63 C65 53.09(16)
C51 P6 C63 C66 174.13(14)
C51 N6 C52 P5 -58.11(17)
C51 N6 C67 C68 54.2(2)
C51 N6 C67 C72 -126.7(2)
C52 P5 C49 N5 -127.58(14)
C52 P5 C53 C54 70.22(14)
C52 P5 C53 C55 -51.00(16)
C52 P5 C53 C56 -173.33(13)
C52 N6 C51 P6 76.46(17)
C52 N6 C67 C68 -173.38(18)
C52 N6 C67 C72 5.7(3)
C53 P5 C49 N5 125.63(14)
C53 P5 C52 N6 -158.54(13)
C57 N5 C49 P5 -137.26(15)
C57 N5 C50 P6 156.25(14)
C57 C58 C59 C60 -0.5(3)
C58 C57 C62 C61 0.8(3)
C58 C59 C60 C61 0.4(3)
C59 C60 C61 C62 0.3(3)
C60 C61 C62 C57 -0.9(3)
C62 C57 C58 C59 -0.1(3)
C63 P6 C50 N5 -160.65(13)
C63 P6 C51 N6 129.92(14)
C67 N6 C51 P6 -149.62(13)
C67 N6 C52 P5 169.05(13)
C67 C68 C69 C70 -1.9(3)
C68 C67 C72 C71 -2.6(3)
C68 C69 C70 C71 -1.2(3)
C69 C70 C71 C72 2.3(3)
C70 C71 C72 C67 -0.4(3)
C72 C67 C68 C69 3.7(3)
