#------------------------------------------------------------------------------
#$Date: 2021-11-10 02:08:40 +0200 (Wed, 10 Nov 2021) $
#$Revision: 270553 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/87/7708755.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_7708755
loop_
_publ_author_name
'Nazarov, Dmitry I.'
'Andronov, Mikhail G.'
'Kuzmin, Aleksey V.'
'Khasanov, Salavat S.'
'Yudanova, Evgeniya I.'
'Shestakov, Alexander F.'
'Otsuka, Akihiro'
'Yamochi, Hideki'
'Kitagawa, Hiroshi'
'Konarev, Dmitri V.'
_publ_section_title
;
 Macrocycle- and metal-centered reduction of metal tetraphenylporphyrins
 where the metal is copper(II), nickel(II) and iron(II).
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15620
_journal_page_last               15632
_journal_paper_doi               10.1039/d1dt02573b
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C44 H28 N4 Ni, C13 H30 P, C7 H8'
_chemical_formula_sum            'C64 H66 N4 Ni P'
_chemical_formula_weight         980.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-23
_audit_creation_method
;
FinalCif V85 by Daniel Kratzert, Freiburg 2021,
https://github.com/dkratzert/FinalCif
;
_audit_update_record
;
2021-07-23 deposited with the CCDC.	2021-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 126.742(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0766(4)
_cell_length_b                   17.4210(3)
_cell_length_c                   27.8842(10)
_cell_measurement_reflns_used    11812
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.1470
_cell_measurement_theta_min      1.8360
_cell_volume                     5090.3(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4566
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -87.00   5.00   1.00  128.00    --  -12.20 -37.00-150.00   92
  2  ω    -76.00  25.00   1.00  128.00    --  -12.20 -19.00 -90.00  101
  3  ω    -67.00 -39.00   1.00  128.00    --  -12.20 -37.00   0.00   28
  4  ω    -30.00  13.00   1.00  128.00    --  -12.20 -57.00 150.00   43
  5  ω    -33.00  -6.00   1.00  128.00    --  -12.20 -57.00   0.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0285037000
_diffrn_orient_matrix_UB_12      0.0035081000
_diffrn_orient_matrix_UB_13      0.0309631000
_diffrn_orient_matrix_UB_21      -0.0204094000
_diffrn_orient_matrix_UB_22      -0.0376710000
_diffrn_orient_matrix_UB_23      0.0001071000
_diffrn_orient_matrix_UB_31      0.0579239000
_diffrn_orient_matrix_UB_32      -0.0150161000
_diffrn_orient_matrix_UB_33      0.0069998000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0859
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.874
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            39961
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.696
_diffrn_reflns_theta_min         1.691
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.459
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       block
_exptl_crystal_F_000             2084
_exptl_crystal_size_max          0.449
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         12628
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1048
_refine_ls_R_factor_gt           0.0592
_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)+(0.0190P)²+5.9448P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1230
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8428
_reflns_number_total             12628
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt02573b2.cif
_cod_data_source_block           exp_1534_int1
_cod_database_code               7708755
_chemical_oxdiff_formula         C65H58N8Ni11P1Br1
_shelx_shelxl_version_number     2018/3
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.027
_oxdiff_exptl_absorpt_empirical_full_min 0.975
_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.
;
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_shelx_estimated_absorpt_t_min   0.821
_shelx_estimated_absorpt_t_max   0.961
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C21A-C210 \\sim C21B-C210
 with sigma of 0.02
 C2-C22B \\sim C1-C22A
 with sigma of 0.02
 C22A-C21A \\sim C22B-C21B
 with sigma of 0.02
 P21-C26A \\sim P21-C26B
 with sigma of 0.02
 C24A-C205 \\sim C24B-C205
 with sigma of 0.02
 C27B-C208 \\sim C27A-C208
 with sigma of 0.02
 C27B-C26B \\sim C27A-C26A
 with sigma of 0.02
 C23B-C202 \\sim C23A-C202
 with sigma of 0.02
 C24B-C23B \\sim C24A-C23A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C23B) = Uanis(C23A)
Uanis(C27B) = Uanis(C27A)
Uanis(C24A) = Uanis(C24B)
Uanis(C26B) = Uanis(C26A)
4. Others
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C21B)=Sof(H21C)=Sof(H21D)=Sof(C22B)=
 Sof(H22C)=Sof(H22D)=Sof(H21G)=Sof(H21H)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(C22A)=
 Sof(H22A)=Sof(H22B)=Sof(H21E)=Sof(H21F)=FVAR(1)
 Sof(C23B)=Sof(H23C)=Sof(H23D)=Sof(C24B)=Sof(H24C)=Sof(H24D)=Sof(H20F)=
 Sof(H20G)=Sof(H20K)=Sof(H20L)=Sof(H20M)=1-FVAR(2)
 Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H20D)=
 Sof(H20E)=Sof(H20H)=Sof(H20I)=Sof(H20J)=FVAR(2)
 Sof(C26B)=Sof(H26C)=Sof(H26D)=Sof(C27B)=Sof(H27C)=Sof(H27D)=Sof(H20P)=
 Sof(H20Q)=1-FVAR(3)
 Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(H20N)=
 Sof(H20O)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C21A(H21A,H21B), C21B(H21C,H21D), C22A(H22A,H22B), C22B(H22C,H22D), C23A(H23A,
 H23B), C23B(H23C,H23D), C24A(H24A,H24B), C24B(H24C,H24D), C26A(H26A,H26B),
 C26B(H26C,H26D), C27A(H27A,H27B), C27B(H27C,H27D), C202(H20D,H20E), C202(H20F,
 H20G), C208(H20N,H20O), C208(H20P,H20Q), C210(H21E,H21F), C210(H21G,H21H)
5.b Aromatic/amide H refined with riding coordinates:
 C103(H103), C104(H104), C108(H108), C109(H109), C113(H113), C114(H114),
 C118(H118), C119(H119), C122(H122), C123(H123), C124(H124), C125(H125),
 C126(H126), C128(H128), C129(H129), C130(H130), C131(H131), C132(H132),
 C134(H134), C135(H135), C136(H136), C137(H137), C138(H138), C140(H140),
 C141(H141), C142(H142), C143(H143), C144(H144), C302(H302), C303(H303),
 C304(H304), C305(H305), C306(H306)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C201(H20A,H20B,H20C), C205(H20H,H20I,H20J),
 C205(H20K,H20L,H20M), C209(H20R,H20S,H20T), C307(H30A,H30B,H30C)
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Ni11 Ni 0.55379(3) 0.60742(2) 0.70237(2) 0.01852(9) Uani 1 1 d . . . . .
N101 N 0.7083(2) 0.56779(13) 0.71161(9) 0.0205(5) Uani 1 1 d . . . . .
N102 N 0.62765(19) 0.57252(12) 0.78619(9) 0.0196(5) Uani 1 1 d . . . . .
N103 N 0.4011(2) 0.64937(12) 0.69431(9) 0.0200(5) Uani 1 1 d . . . . .
N104 N 0.4806(2) 0.64298(12) 0.61925(9) 0.0205(5) Uani 1 1 d . . . . .
C101 C 0.6493(2) 0.59935(15) 0.61157(12) 0.0213(6) Uani 1 1 d . . . . .
C102 C 0.7312(2) 0.56856(15) 0.66906(11) 0.0202(6) Uani 1 1 d . . . . .
C103 C 0.8517(3) 0.53388(16) 0.69255(12) 0.0254(6) Uani 1 1 d . . . . .
H103 H 0.888730 0.527777 0.672087 0.030 Uiso 1 1 calc R U . . .
C104 C 0.9032(2) 0.51140(16) 0.74899(12) 0.0238(6) Uani 1 1 d . . . . .
H104 H 0.983014 0.486559 0.775787 0.029 Uiso 1 1 calc R U . . .
C105 C 0.8134(2) 0.53241(15) 0.76081(11) 0.0196(5) Uani 1 1 d . . . . .
C106 C 0.8302(2) 0.51625(15) 0.81436(11) 0.0206(6) Uani 1 1 d . . . . .
C107 C 0.7418(2) 0.53444(15) 0.82543(11) 0.0186(5) Uani 1 1 d . . . . .
C108 C 0.7585(2) 0.51765(15) 0.88027(11) 0.0216(6) Uani 1 1 d . . . . .
H108 H 0.828494 0.491394 0.914034 0.026 Uiso 1 1 calc R U . . .
C109 C 0.6561(2) 0.54621(15) 0.87465(11) 0.0205(6) Uani 1 1 d . . . . .
H109 H 0.640198 0.543446 0.903679 0.025 Uiso 1 1 calc R U . . .
C110 C 0.5753(2) 0.58163(15) 0.81670(11) 0.0189(5) Uani 1 1 d . . . . .
C111 C 0.4606(2) 0.61916(15) 0.79481(11) 0.0202(6) Uani 1 1 d . . . . .
C112 C 0.3792(2) 0.65067(15) 0.73724(11) 0.0194(5) Uani 1 1 d . . . . .
C113 C 0.2609(3) 0.68952(15) 0.71403(12) 0.0236(6) Uani 1 1 d . . . . .
H113 H 0.225475 0.698732 0.734900 0.028 Uiso 1 1 calc R U . . .
C114 C 0.2097(3) 0.71043(15) 0.65737(12) 0.0231(6) Uani 1 1 d . . . . .
H114 H 0.130840 0.736262 0.630588 0.028 Uiso 1 1 calc R U . . .
C115 C 0.2970(2) 0.68628(15) 0.64505(12) 0.0205(6) Uani 1 1 d . . . . .
C116 C 0.2790(2) 0.70038(15) 0.59103(11) 0.0211(6) Uani 1 1 d . . . . .
C117 C 0.3649(2) 0.67984(15) 0.57943(11) 0.0202(6) Uani 1 1 d . . . . .
C118 C 0.3449(3) 0.69274(16) 0.52331(12) 0.0240(6) Uani 1 1 d . . . . .
H118 H 0.273095 0.716965 0.488913 0.029 Uiso 1 1 calc R U . . .
C119 C 0.4470(3) 0.66406(16) 0.52868(11) 0.0235(6) Uani 1 1 d . . . . .
H119 H 0.460355 0.663960 0.498733 0.028 Uiso 1 1 calc R U . . .
C120 C 0.5320(2) 0.63359(15) 0.58837(11) 0.0206(6) Uani 1 1 d . . . . .
C121 C 0.6885(2) 0.59446(16) 0.57069(11) 0.0219(6) Uani 1 1 d . . . . .
C122 C 0.6813(3) 0.52597(17) 0.54348(12) 0.0259(6) Uani 1 1 d . . . . .
H122 H 0.651688 0.481027 0.550931 0.031 Uiso 1 1 calc R U . . .
C123 C 0.7168(3) 0.52212(17) 0.50541(12) 0.0282(6) Uani 1 1 d . . . . .
H123 H 0.710347 0.475007 0.486623 0.034 Uiso 1 1 calc R U . . .
C124 C 0.7615(3) 0.58714(18) 0.49507(13) 0.0299(7) Uani 1 1 d . . . . .
H124 H 0.787723 0.584495 0.469879 0.036 Uiso 1 1 calc R U . . .
C125 C 0.7679(3) 0.65592(18) 0.52131(13) 0.0321(7) Uani 1 1 d . . . . .
H125 H 0.797100 0.700812 0.513556 0.039 Uiso 1 1 calc R U . . .
C126 C 0.7319(3) 0.65953(17) 0.55897(13) 0.0292(7) Uani 1 1 d . . . . .
H126 H 0.736860 0.707021 0.576997 0.035 Uiso 1 1 calc R U . . .
C127 C 0.9513(2) 0.47654(16) 0.86292(11) 0.0222(6) Uani 1 1 d . . . . .
C128 C 0.9489(3) 0.40230(17) 0.88082(12) 0.0273(6) Uani 1 1 d . . . . .
H128 H 0.869615 0.376517 0.862258 0.033 Uiso 1 1 calc R U . . .
C129 C 1.0612(3) 0.36562(18) 0.92550(12) 0.0305(7) Uani 1 1 d . . . . .
H129 H 1.058174 0.315169 0.937533 0.037 Uiso 1 1 calc R U . . .
C130 C 1.1773(3) 0.40213(18) 0.95255(12) 0.0316(7) Uani 1 1 d . . . . .
H130 H 1.254137 0.376517 0.982521 0.038 Uiso 1 1 calc R U . . .
C131 C 1.1810(3) 0.47588(19) 0.93585(13) 0.0334(7) Uani 1 1 d . . . . .
H131 H 1.260622 0.501388 0.954619 0.040 Uiso 1 1 calc R U . . .
C132 C 1.0687(3) 0.51308(17) 0.89159(12) 0.0262(6) Uani 1 1 d . . . . .
H132 H 1.072170 0.564205 0.880775 0.031 Uiso 1 1 calc R U . . .
C133 C 0.4220(3) 0.62873(16) 0.83530(12) 0.0241(6) Uani 1 1 d . . . . .
C134 C 0.3065(3) 0.60039(18) 0.81981(13) 0.0313(7) Uani 1 1 d . . . . .
H134 H 0.253608 0.571296 0.784107 0.038 Uiso 1 1 calc R U . . .
C135 C 0.2670(3) 0.6138(2) 0.85545(15) 0.0408(8) Uani 1 1 d . . . . .
H135 H 0.186964 0.594649 0.843622 0.049 Uiso 1 1 calc R U . . .
C136 C 0.3435(3) 0.6546(2) 0.90798(15) 0.0439(9) Uani 1 1 d . . . . .
H136 H 0.316168 0.664071 0.932273 0.053 Uiso 1 1 calc R U . . .
C137 C 0.4596(3) 0.68166(18) 0.92493(14) 0.0381(8) Uani 1 1 d . . . . .
H137 H 0.513491 0.708757 0.961596 0.046 Uiso 1 1 calc R U . . .
C138 C 0.4988(3) 0.66972(17) 0.88899(12) 0.0291(7) Uani 1 1 d . . . . .
H138 H 0.578503 0.689559 0.900933 0.035 Uiso 1 1 calc R U . . .
C139 C 0.1574(2) 0.73911(16) 0.54224(11) 0.0213(6) Uani 1 1 d . . . . .
C140 C 0.0427(3) 0.69879(16) 0.50884(12) 0.0252(6) Uani 1 1 d . . . . .
H140 H 0.041450 0.646135 0.517326 0.030 Uiso 1 1 calc R U . . .
C141 C -0.0697(3) 0.73436(17) 0.46339(12) 0.0260(6) Uani 1 1 d . . . . .
H141 H -0.146926 0.705817 0.440987 0.031 Uiso 1 1 calc R U . . .
C142 C -0.0704(3) 0.81070(17) 0.45044(12) 0.0276(6) Uani 1 1 d . . . . .
H142 H -0.147744 0.834970 0.419489 0.033 Uiso 1 1 calc R U . . .
C143 C 0.0429(3) 0.85186(17) 0.48298(13) 0.0299(7) Uani 1 1 d . . . . .
H143 H 0.043237 0.904481 0.474154 0.036 Uiso 1 1 calc R U . . .
C144 C 0.1554(3) 0.81649(16) 0.52830(12) 0.0251(6) Uani 1 1 d . . . . .
H144 H 0.232492 0.845220 0.550269 0.030 Uiso 1 1 calc R U . . .
P21 P 0.41087(7) 0.36053(5) 0.74624(3) 0.02847(18) Uani 1 1 d D . . . .
C1 C 0.0487(6) 0.5286(4) 0.6354(3) 0.0352(17) Uani 0.529(6) 1 d D . P A 1
H1A H -0.002557 0.574336 0.614160 0.053 Uiso 0.529(6) 1 calc R U P A 1
H1B H 0.106948 0.539376 0.678397 0.053 Uiso 0.529(6) 1 calc R U P A 1
H1C H -0.007709 0.485956 0.628247 0.053 Uiso 0.529(6) 1 calc R U P A 1
C2 C 0.0854(11) 0.5045(7) 0.5854(4) 0.047(3) Uani 0.471(6) 1 d D . P A 2
H2A H 0.169993 0.520564 0.598051 0.070 Uiso 0.471(6) 1 calc R U P A 2
H2B H 0.022236 0.543506 0.558883 0.070 Uiso 0.471(6) 1 calc R U P A 2
H2C H 0.062711 0.455481 0.564069 0.070 Uiso 0.471(6) 1 calc R U P A 2
C21A C 0.2062(5) 0.4342(3) 0.6422(2) 0.0253(14) Uani 0.529(6) 1 d D . P A 1
H21A H 0.149548 0.391422 0.635940 0.030 Uiso 0.529(6) 1 calc R U P A 1
H21B H 0.245246 0.420595 0.622023 0.030 Uiso 0.529(6) 1 calc R U P A 1
C21B C 0.1703(5) 0.4294(4) 0.6803(3) 0.0342(18) Uani 0.471(6) 1 d D . P A 2
H21C H 0.159814 0.423349 0.712402 0.041 Uiso 0.471(6) 1 calc R U P A 2
H21D H 0.141737 0.381241 0.656754 0.041 Uiso 0.471(6) 1 calc R U P A 2
C22A C 0.1250(7) 0.5072(4) 0.6129(3) 0.0272(16) Uani 0.529(6) 1 d D . P A 1
H22A H 0.181980 0.550526 0.620552 0.033 Uiso 0.529(6) 1 calc R U P A 1
H22B H 0.065638 0.499368 0.569086 0.033 Uiso 0.529(6) 1 calc R U P A 1
C22B C 0.0873(7) 0.4951(4) 0.6398(3) 0.0323(18) Uani 0.471(6) 1 d D . P A 2
H22C H -0.001108 0.486619 0.626374 0.039 Uiso 0.471(6) 1 calc R U P A 2
H22D H 0.118406 0.543409 0.663165 0.039 Uiso 0.471(6) 1 calc R U P A 2
C23A C 0.5110(3) 0.3793(2) 0.68267(15) 0.0306(8) Uani 0.864(4) 1 d D . P B 1
H23A H 0.440367 0.343938 0.654630 0.037 Uiso 0.864(4) 1 calc R U P B 1
H23B H 0.479876 0.432483 0.669467 0.037 Uiso 0.864(4) 1 calc R U P B 1
C23B C 0.5986(19) 0.3514(12) 0.7155(8) 0.0306(8) Uani 0.136(4) 1 d D . P B 2
H23C H 0.588698 0.296143 0.705434 0.037 Uiso 0.136(4) 1 calc R U P B 2
H23D H 0.690636 0.364081 0.740288 0.037 Uiso 0.136(4) 1 calc R U P B 2
C24A C 0.6215(3) 0.3651(2) 0.68012(14) 0.0295(8) Uani 0.864(4) 1 d D . P B 1
H24A H 0.695337 0.397023 0.710494 0.035 Uiso 0.864(4) 1 calc R U P B 1
H24B H 0.647365 0.310513 0.689009 0.035 Uiso 0.864(4) 1 calc R U P B 1
C24B C 0.5280(19) 0.3984(13) 0.6589(8) 0.0295(8) Uani 0.136(4) 1 d D . P B 2
H24C H 0.535848 0.453472 0.669416 0.035 Uiso 0.136(4) 1 calc R U P B 2
H24D H 0.436335 0.384797 0.634218 0.035 Uiso 0.136(4) 1 calc R U P B 2
C26A C 0.4668(3) 0.3608(2) 0.82402(14) 0.0291(8) Uani 0.846(4) 1 d D . P C 1
H26A H 0.523893 0.316262 0.844952 0.035 Uiso 0.846(4) 1 calc R U P C 1
H26B H 0.517559 0.407940 0.843802 0.035 Uiso 0.846(4) 1 calc R U P C 1
C26B C 0.3931(18) 0.3242(10) 0.7999(7) 0.0291(8) Uani 0.154(4) 1 d D . P C 2
H26C H 0.301976 0.313700 0.781012 0.035 Uiso 0.154(4) 1 calc R U P C 2
H26D H 0.441132 0.275518 0.816754 0.035 Uiso 0.154(4) 1 calc R U P C 2
C27A C 0.3590(4) 0.3575(3) 0.83086(16) 0.0416(10) Uani 0.846(4) 1 d D . P C 1
H27A H 0.301970 0.402259 0.810478 0.050 Uiso 0.846(4) 1 calc R U P C 1
H27B H 0.307975 0.310390 0.811394 0.050 Uiso 0.846(4) 1 calc R U P C 1
C27B C 0.444(2) 0.3838(12) 0.8499(8) 0.0416(10) Uani 0.154(4) 1 d D . P C 2
H27C H 0.405073 0.434380 0.832126 0.050 Uiso 0.154(4) 1 calc R U P C 2
H27D H 0.537854 0.388886 0.872165 0.050 Uiso 0.154(4) 1 calc R U P C 2
C201 C 0.3283(3) 0.27571(18) 0.71003(15) 0.0458(9) Uani 1 1 d . . . . .
H20A H 0.310326 0.273428 0.670517 0.069 Uiso 1 1 calc R U . . .
H20B H 0.247892 0.274750 0.705373 0.069 Uiso 1 1 calc R U . . .
H20C H 0.380597 0.231459 0.733923 0.069 Uiso 1 1 calc R U . . .
C202 C 0.5494(3) 0.36716(18) 0.74822(14) 0.0347(7) Uani 1 1 d D . . . .
H20D H 0.602747 0.410734 0.774025 0.042 Uiso 0.864(4) 1 calc R U P B 1
H20E H 0.600368 0.319584 0.765703 0.042 Uiso 0.864(4) 1 calc R U P B 1
H20F H 0.570082 0.422375 0.757203 0.042 Uiso 0.136(4) 1 calc R U P B 2
H20G H 0.613280 0.340915 0.786522 0.042 Uiso 0.136(4) 1 calc R U P B 2
C205 C 0.5824(3) 0.38486(19) 0.61903(14) 0.0397(8) Uani 1 1 d D . . . .
H20H H 0.509888 0.352787 0.589185 0.060 Uiso 0.864(4) 1 calc R U P B 1
H20I H 0.654099 0.375665 0.617289 0.060 Uiso 0.864(4) 1 calc R U P B 1
H20J H 0.557776 0.439072 0.610621 0.060 Uiso 0.864(4) 1 calc R U P B 1
H20K H 0.535685 0.417986 0.583595 0.060 Uiso 0.136(4) 1 calc R U P B 2
H20L H 0.570336 0.331039 0.606486 0.060 Uiso 0.136(4) 1 calc R U P B 2
H20M H 0.673511 0.397547 0.643429 0.060 Uiso 0.136(4) 1 calc R U P B 2
C208 C 0.4113(3) 0.3576(2) 0.89626(14) 0.0441(8) Uani 1 1 d D . . . .
H20N H 0.338536 0.349773 0.897969 0.053 Uiso 0.846(4) 1 calc R U P C 1
H20O H 0.467944 0.312494 0.915487 0.053 Uiso 0.846(4) 1 calc R U P C 1
H20P H 0.319161 0.358936 0.878270 0.053 Uiso 0.154(4) 1 calc R U P C 2
H20Q H 0.450021 0.308102 0.916629 0.053 Uiso 0.154(4) 1 calc R U P C 2
C209 C 0.4835(4) 0.4263(2) 0.93358(15) 0.0488(9) Uani 1 1 d . . . . .
H20R H 0.435278 0.472964 0.912412 0.073 Uiso 1 1 calc R U . . .
H20S H 0.566805 0.428204 0.941014 0.073 Uiso 1 1 calc R U . . .
H20T H 0.495832 0.422937 0.971815 0.073 Uiso 1 1 calc R U . . .
C210 C 0.3100(3) 0.44255(17) 0.70814(13) 0.0301(7) Uani 1 1 d D . . . .
H21E H 0.269845 0.456338 0.727815 0.036 Uiso 0.529(6) 1 calc R U P A 1
H21F H 0.364911 0.486179 0.713914 0.036 Uiso 0.529(6) 1 calc R U P A 1
H21G H 0.341550 0.485527 0.736963 0.036 Uiso 0.471(6) 1 calc R U P A 2
H21H H 0.317642 0.458342 0.676282 0.036 Uiso 0.471(6) 1 calc R U P A 2
C301 C 1.0013(3) 0.27388(19) 0.73945(13) 0.0331(7) Uani 1 1 d . . . . .
C302 C 1.0595(3) 0.21888(18) 0.72763(14) 0.0352(7) Uani 1 1 d . . . . .
H302 H 1.116049 0.182925 0.757818 0.042 Uiso 1 1 calc R U . . .
C303 C 1.0368(3) 0.21550(17) 0.67260(14) 0.0322(7) Uani 1 1 d . . . . .
H303 H 1.077631 0.177292 0.665227 0.039 Uiso 1 1 calc R U . . .
C304 C 0.9557(3) 0.26677(18) 0.62849(13) 0.0327(7) Uani 1 1 d . . . . .
H304 H 0.939387 0.263906 0.590451 0.039 Uiso 1 1 calc R U . . .
C305 C 0.8980(3) 0.32256(19) 0.63981(14) 0.0387(8) Uani 1 1 d . . . . .
H305 H 0.842672 0.358877 0.609675 0.046 Uiso 1 1 calc R U . . .
C306 C 0.9205(3) 0.32583(19) 0.69508(14) 0.0376(8) Uani 1 1 d . . . . .
H306 H 0.879807 0.364213 0.702450 0.045 Uiso 1 1 calc R U . . .
C307 C 1.0269(4) 0.2785(3) 0.79993(15) 0.0585(11) Uani 1 1 d . . . . .
H30A H 1.035155 0.226609 0.815373 0.088 Uiso 1 1 calc R U . . .
H30B H 0.956046 0.305067 0.795883 0.088 Uiso 1 1 calc R U . . .
H30C H 1.106257 0.306995 0.827730 0.088 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'
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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.0343
0 1 0 0.0539
0 0 1 0.0769
1 0 -2 0.1560
-1 0 2 0.1499
0 0 -1 0.0820
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
N101 Ni11 N102 90.01(8) . . ?
N101 Ni11 N103 178.64(9) . . ?
N101 Ni11 N104 90.15(8) . . ?
N103 Ni11 N102 89.66(8) . . ?
N104 Ni11 N102 179.56(9) . . ?
N104 Ni11 N103 90.17(8) . . ?
C102 N101 Ni11 127.23(17) . . ?
C105 N101 Ni11 127.74(16) . . ?
C105 N101 C102 105.0(2) . . ?
C107 N102 Ni11 127.16(16) . . ?
C107 N102 C110 105.4(2) . . ?
C110 N102 Ni11 127.46(17) . . ?
C112 N103 Ni11 127.85(17) . . ?
C115 N103 Ni11 127.00(16) . . ?
C115 N103 C112 105.1(2) . . ?
C117 N104 Ni11 127.38(16) . . ?
C120 N104 Ni11 127.54(17) . . ?
C120 N104 C117 105.0(2) . . ?
C102 C101 C121 118.2(2) . . ?
C120 C101 C102 125.0(2) . . ?
C120 C101 C121 116.8(2) . . ?
N101 C102 C101 125.1(2) . . ?
N101 C102 C103 110.3(2) . . ?
C101 C102 C103 124.5(2) . . ?
C102 C103 H103 126.2 . . ?
C104 C103 C102 107.6(2) . . ?
C104 C103 H103 126.2 . . ?
C103 C104 H104 126.7 . . ?
C103 C104 C105 106.7(2) . . ?
C105 C104 H104 126.7 . . ?
N101 C105 C104 110.4(2) . . ?
N101 C105 C106 125.3(2) . . ?
C106 C105 C104 124.2(2) . . ?
C105 C106 C127 117.5(2) . . ?
C107 C106 C105 124.5(2) . . ?
C107 C106 C127 118.0(2) . . ?
N102 C107 C106 125.3(2) . . ?
N102 C107 C108 110.1(2) . . ?
C106 C107 C108 124.6(2) . . ?
C107 C108 H108 126.5 . . ?
C109 C108 C107 107.0(2) . . ?
C109 C108 H108 126.5 . . ?
C108 C109 H109 126.3 . . ?
C108 C109 C110 107.5(2) . . ?
C110 C109 H109 126.3 . . ?
N102 C110 C109 109.9(2) . . ?
N102 C110 C111 125.6(2) . . ?
C111 C110 C109 124.5(2) . . ?
C110 C111 C112 124.3(2) . . ?
C110 C111 C133 118.7(2) . . ?
C112 C111 C133 116.9(2) . . ?
N103 C112 C111 125.1(2) . . ?
N103 C112 C113 109.9(2) . . ?
C111 C112 C113 125.0(2) . . ?
C112 C113 H113 126.2 . . ?
C114 C113 C112 107.5(2) . . ?
C114 C113 H113 126.2 . . ?
C113 C114 H114 126.5 . . ?
C113 C114 C115 107.0(2) . . ?
C115 C114 H114 126.5 . . ?
N103 C115 C114 110.4(2) . . ?
N103 C115 C116 125.5(2) . . ?
C116 C115 C114 124.0(2) . . ?
C115 C116 C139 117.3(2) . . ?
C117 C116 C115 124.5(2) . . ?
C117 C116 C139 118.1(2) . . ?
N104 C117 C116 125.4(2) . . ?
N104 C117 C118 110.1(2) . . ?
C116 C117 C118 124.5(2) . . ?
C117 C118 H118 126.4 . . ?
C119 C118 C117 107.3(2) . . ?
C119 C118 H118 126.4 . . ?
C118 C119 H119 126.4 . . ?
C118 C119 C120 107.1(2) . . ?
C120 C119 H119 126.4 . . ?
N104 C120 C101 124.9(2) . . ?
N104 C120 C119 110.4(2) . . ?
C101 C120 C119 124.7(2) . . ?
C122 C121 C101 121.3(2) . . ?
C122 C121 C126 118.5(2) . . ?
C126 C121 C101 120.2(2) . . ?
C121 C122 H122 119.5 . . ?
C121 C122 C123 120.9(3) . . ?
C123 C122 H122 119.5 . . ?
C122 C123 H123 120.2 . . ?
C124 C123 C122 119.7(3) . . ?
C124 C123 H123 120.2 . . ?
C123 C124 H124 120.0 . . ?
C125 C124 C123 120.1(3) . . ?
C125 C124 H124 120.0 . . ?
C124 C125 H125 120.0 . . ?
C124 C125 C126 120.0(3) . . ?
C126 C125 H125 120.0 . . ?
C121 C126 H126 119.6 . . ?
C125 C126 C121 120.8(3) . . ?
C125 C126 H126 119.6 . . ?
C128 C127 C106 120.8(2) . . ?
C132 C127 C106 120.9(2) . . ?
C132 C127 C128 118.2(3) . . ?
C127 C128 H128 119.7 . . ?
C129 C128 C127 120.7(3) . . ?
C129 C128 H128 119.7 . . ?
C128 C129 H129 119.8 . . ?
C130 C129 C128 120.3(3) . . ?
C130 C129 H129 119.8 . . ?
C129 C130 H130 120.2 . . ?
C131 C130 C129 119.6(3) . . ?
C131 C130 H130 120.2 . . ?
C130 C131 H131 119.9 . . ?
C130 C131 C132 120.2(3) . . ?
C132 C131 H131 119.9 . . ?
C127 C132 C131 120.9(3) . . ?
C127 C132 H132 119.5 . . ?
C131 C132 H132 119.5 . . ?
C134 C133 C111 121.3(3) . . ?
C134 C133 C138 117.6(2) . . ?
C138 C133 C111 121.0(2) . . ?
C133 C134 H134 119.4 . . ?
C135 C134 C133 121.3(3) . . ?
C135 C134 H134 119.4 . . ?
C134 C135 H135 119.9 . . ?
C136 C135 C134 120.3(3) . . ?
C136 C135 H135 119.9 . . ?
C135 C136 H136 120.3 . . ?
C137 C136 C135 119.4(3) . . ?
C137 C136 H136 120.3 . . ?
C136 C137 H137 119.7 . . ?
C136 C137 C138 120.6(3) . . ?
C138 C137 H137 119.7 . . ?
C133 C138 H138 119.6 . . ?
C137 C138 C133 120.7(3) . . ?
C137 C138 H138 119.6 . . ?
C140 C139 C116 120.9(2) . . ?
C140 C139 C144 117.8(2) . . ?
C144 C139 C116 121.3(2) . . ?
C139 C140 H140 119.5 . . ?
C141 C140 C139 121.0(3) . . ?
C141 C140 H140 119.5 . . ?
C140 C141 H141 119.7 . . ?
C142 C141 C140 120.6(3) . . ?
C142 C141 H141 119.7 . . ?
C141 C142 H142 120.3 . . ?
C141 C142 C143 119.4(3) . . ?
C143 C142 H142 120.3 . . ?
C142 C143 H143 119.9 . . ?
C144 C143 C142 120.2(3) . . ?
C144 C143 H143 119.9 . . ?
C139 C144 H144 119.5 . . ?
C143 C144 C139 121.0(3) . . ?
C143 C144 H144 119.5 . . ?
C26B P21 C202 130.1(6) . . ?
C26B P21 C210 111.4(6) . . ?
C201 P21 C26A 110.97(17) . . ?
C201 P21 C26B 80.7(6) . . ?
C201 P21 C202 109.69(16) . . ?
C201 P21 C210 110.42(15) . . ?
C202 P21 C26A 106.57(15) . . ?
C202 P21 C210 109.83(14) . . ?
C210 P21 C26A 109.28(15) . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C22A C1 H1A 109.5 . . ?
C22A C1 H1B 109.5 . . ?
C22A C1 H1C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C22B C2 H2A 109.5 . . ?
C22B C2 H2B 109.5 . . ?
C22B C2 H2C 109.5 . . ?
H21A C21A H21B 107.7 . . ?
C22A C21A H21A 108.8 . . ?
C22A C21A H21B 108.8 . . ?
C210 C21A H21A 108.8 . . ?
C210 C21A H21B 108.8 . . ?
C210 C21A C22A 113.7(4) . . ?
H21C C21B H21D 107.9 . . ?
C22B C21B H21C 109.2 . . ?
C22B C21B H21D 109.2 . . ?
C210 C21B H21C 109.2 . . ?
C210 C21B H21D 109.2 . . ?
C210 C21B C22B 112.0(5) . . ?
C1 C22A C21A 113.6(6) . . ?
C1 C22A H22A 108.8 . . ?
C1 C22A H22B 108.8 . . ?
C21A C22A H22A 108.8 . . ?
C21A C22A H22B 108.8 . . ?
H22A C22A H22B 107.7 . . ?
C2 C22B C21B 113.8(7) . . ?
C2 C22B H22C 108.8 . . ?
C2 C22B H22D 108.8 . . ?
C21B C22B H22C 108.8 . . ?
C21B C22B H22D 108.8 . . ?
H22C C22B H22D 107.7 . . ?
H23A C23A H23B 107.9 . . ?
C24A C23A H23A 109.2 . . ?
C24A C23A H23B 109.2 . . ?
C24A C23A C202 112.3(3) . . ?
C202 C23A H23A 109.2 . . ?
C202 C23A H23B 109.2 . . ?
H23C C23B H23D 108.2 . . ?
C24B C23B H23C 109.7 . . ?
C24B C23B H23D 109.7 . . ?
C202 C23B H23C 109.7 . . ?
C202 C23B H23D 109.7 . . ?
C202 C23B C24B 109.8(13) . . ?
C23A C24A H24A 109.8 . . ?
C23A C24A H24B 109.8 . . ?
H24A C24A H24B 108.3 . . ?
C205 C24A C23A 109.4(3) . . ?
C205 C24A H24A 109.8 . . ?
C205 C24A H24B 109.8 . . ?
C23B C24B H24C 109.1 . . ?
C23B C24B H24D 109.1 . . ?
C23B C24B C205 112.7(12) . . ?
H24C C24B H24D 107.8 . . ?
C205 C24B H24C 109.1 . . ?
C205 C24B H24D 109.1 . . ?
P21 C26A H26A 108.8 . . ?
P21 C26A H26B 108.8 . . ?
H26A C26A H26B 107.7 . . ?
C27A C26A P21 113.8(2) . . ?
C27A C26A H26A 108.8 . . ?
C27A C26A H26B 108.8 . . ?
P21 C26B H26C 110.0 . . ?
P21 C26B H26D 110.0 . . ?
H26C C26B H26D 108.3 . . ?
C27B C26B P21 108.6(11) . . ?
C27B C26B H26C 110.0 . . ?
C27B C26B H26D 110.0 . . ?
C26A C27A H27A 109.4 . . ?
C26A C27A H27B 109.4 . . ?
H27A C27A H27B 108.0 . . ?
C208 C27A C26A 111.3(3) . . ?
C208 C27A H27A 109.4 . . ?
C208 C27A H27B 109.4 . . ?
C26B C27B H27C 109.6 . . ?
C26B C27B H27D 109.6 . . ?
C26B C27B C208 110.3(12) . . ?
H27C C27B H27D 108.1 . . ?
C208 C27B H27C 109.6 . . ?
C208 C27B H27D 109.6 . . ?
P21 C201 H20A 109.5 . . ?
P21 C201 H20B 109.5 . . ?
P21 C201 H20C 109.5 . . ?
H20A C201 H20B 109.5 . . ?
H20A C201 H20C 109.5 . . ?
H20B C201 H20C 109.5 . . ?
P21 C202 H20D 109.5 . . ?
P21 C202 H20E 109.5 . . ?
P21 C202 H20F 100.9 . . ?
P21 C202 H20G 100.9 . . ?
C23A C202 P21 110.9(2) . . ?
C23A C202 H20D 109.5 . . ?
C23A C202 H20E 109.5 . . ?
C23B C202 P21 144.0(9) . . ?
C23B C202 H20F 100.9 . . ?
C23B C202 H20G 100.9 . . ?
H20D C202 H20E 108.1 . . ?
H20F C202 H20G 104.4 . . ?
C24A C205 H20H 109.5 . . ?
C24A C205 H20I 109.5 . . ?
C24A C205 H20J 109.5 . . ?
C24B C205 H20K 109.5 . . ?
C24B C205 H20L 109.5 . . ?
C24B C205 H20M 109.5 . . ?
H20H C205 H20I 109.5 . . ?
H20H C205 H20J 109.5 . . ?
H20I C205 H20J 109.5 . . ?
H20K C205 H20L 109.5 . . ?
H20K C205 H20M 109.5 . . ?
H20L C205 H20M 109.5 . . ?
C27A C208 H20N 107.6 . . ?
C27A C208 H20O 107.6 . . ?
C27B C208 H20P 113.9 . . ?
C27B C208 H20Q 113.9 . . ?
H20N C208 H20O 107.1 . . ?
H20P C208 H20Q 111.1 . . ?
C209 C208 C27A 118.8(3) . . ?
C209 C208 C27B 88.4(7) . . ?
C209 C208 H20N 107.6 . . ?
C209 C208 H20O 107.6 . . ?
C209 C208 H20P 113.9 . . ?
C209 C208 H20Q 113.9 . . ?
C208 C209 H20R 109.5 . . ?
C208 C209 H20S 109.5 . . ?
C208 C209 H20T 109.5 . . ?
H20R C209 H20S 109.5 . . ?
H20R C209 H20T 109.5 . . ?
H20S C209 H20T 109.5 . . ?
P21 C210 H21E 108.1 . . ?
P21 C210 H21F 108.1 . . ?
P21 C210 H21G 108.6 . . ?
P21 C210 H21H 108.6 . . ?
C21A C210 P21 116.9(3) . . ?
C21A C210 H21E 108.1 . . ?
C21A C210 H21F 108.1 . . ?
C21B C210 P21 114.6(3) . . ?
C21B C210 H21G 108.6 . . ?
C21B C210 H21H 108.6 . . ?
H21E C210 H21F 107.3 . . ?
H21G C210 H21H 107.6 . . ?
C302 C301 C307 121.1(3) . . ?
C306 C301 C302 118.5(3) . . ?
C306 C301 C307 120.3(3) . . ?
C301 C302 H302 119.6 . . ?
C303 C302 C301 120.8(3) . . ?
C303 C302 H302 119.6 . . ?
C302 C303 H303 119.7 . . ?
C304 C303 C302 120.5(3) . . ?
C304 C303 H303 119.7 . . ?
C303 C304 H304 120.3 . . ?
C303 C304 C305 119.4(3) . . ?
C305 C304 H304 120.3 . . ?
C304 C305 H305 119.9 . . ?
C304 C305 C306 120.2(3) . . ?
C306 C305 H305 119.9 . . ?
C301 C306 C305 120.6(3) . . ?
C301 C306 H306 119.7 . . ?
C305 C306 H306 119.7 . . ?
C301 C307 H30A 109.5 . . ?
C301 C307 H30B 109.5 . . ?
C301 C307 H30C 109.5 . . ?
H30A C307 H30B 109.5 . . ?
H30A C307 H30C 109.5 . . ?
H30B C307 H30C 109.5 . . ?
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
Ni11 N101 2.001(2) . ?
Ni11 N102 2.016(2) . ?
Ni11 N103 2.009(2) . ?
Ni11 N104 2.004(2) . ?
N101 C102 1.387(3) . ?
N101 C105 1.377(3) . ?
N102 C107 1.382(3) . ?
N102 C110 1.383(3) . ?
N103 C112 1.387(3) . ?
N103 C115 1.384(3) . ?
N104 C117 1.387(3) . ?
N104 C120 1.384(3) . ?
C101 C102 1.397(4) . ?
C101 C120 1.392(4) . ?
C101 C121 1.507(3) . ?
C102 C103 1.428(4) . ?
C103 H103 0.9500 . ?
C103 C104 1.348(4) . ?
C104 H104 0.9500 . ?
C104 C105 1.443(3) . ?
C105 C106 1.402(3) . ?
C106 C107 1.400(3) . ?
C106 C127 1.502(4) . ?
C107 C108 1.439(3) . ?
C108 H108 0.9500 . ?
C108 C109 1.347(4) . ?
C109 H109 0.9500 . ?
C109 C110 1.437(3) . ?
C110 C111 1.399(3) . ?
C111 C112 1.402(3) . ?
C111 C133 1.496(3) . ?
C112 C113 1.440(4) . ?
C113 H113 0.9500 . ?
C113 C114 1.346(4) . ?
C114 H114 0.9500 . ?
C114 C115 1.437(4) . ?
C115 C116 1.401(3) . ?
C116 C117 1.389(4) . ?
C116 C139 1.499(4) . ?
C117 C118 1.442(3) . ?
C118 H118 0.9500 . ?
C118 C119 1.347(4) . ?
C119 H119 0.9500 . ?
C119 C120 1.440(4) . ?
C121 C122 1.386(4) . ?
C121 C126 1.391(4) . ?
C122 H122 0.9500 . ?
C122 C123 1.391(4) . ?
C123 H123 0.9500 . ?
C123 C124 1.382(4) . ?
C124 H124 0.9500 . ?
C124 C125 1.380(4) . ?
C125 H125 0.9500 . ?
C125 C126 1.386(4) . ?
C126 H126 0.9500 . ?
C127 C128 1.394(4) . ?
C127 C132 1.390(4) . ?
C128 H128 0.9500 . ?
C128 C129 1.389(4) . ?
C129 H129 0.9500 . ?
C129 C130 1.381(4) . ?
C130 H130 0.9500 . ?
C130 C131 1.378(4) . ?
C131 H131 0.9500 . ?
C131 C132 1.390(4) . ?
C132 H132 0.9500 . ?
C133 C134 1.390(4) . ?
C133 C138 1.400(4) . ?
C134 H134 0.9500 . ?
C134 C135 1.387(4) . ?
C135 H135 0.9500 . ?
C135 C136 1.378(5) . ?
C136 H136 0.9500 . ?
C136 C137 1.376(5) . ?
C137 H137 0.9500 . ?
C137 C138 1.387(4) . ?
C138 H138 0.9500 . ?
C139 C140 1.393(4) . ?
C139 C144 1.399(4) . ?
C140 H140 0.9500 . ?
C140 C141 1.386(4) . ?
C141 H141 0.9500 . ?
C141 C142 1.377(4) . ?
C142 H142 0.9500 . ?
C142 C143 1.387(4) . ?
C143 H143 0.9500 . ?
C143 C144 1.385(4) . ?
C144 H144 0.9500 . ?
P21 C26A 1.828(3) . ?
P21 C26B 1.764(13) . ?
P21 C201 1.750(3) . ?
P21 C202 1.783(3) . ?
P21 C210 1.798(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C22A 1.507(9) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C2 C22B 1.510(9) . ?
C21A H21A 0.9900 . ?
C21A H21B 0.9900 . ?
C21A C22A 1.541(8) . ?
C21A C210 1.502(5) . ?
C21B H21C 0.9900 . ?
C21B H21D 0.9900 . ?
C21B C22B 1.516(9) . ?
C21B C210 1.516(6) . ?
C22A H22A 0.9900 . ?
C22A H22B 0.9900 . ?
C22B H22C 0.9900 . ?
C22B H22D 0.9900 . ?
C23A H23A 0.9900 . ?
C23A H23B 0.9900 . ?
C23A C24A 1.509(4) . ?
C23A C202 1.594(4) . ?
C23B H23C 0.9900 . ?
C23B H23D 0.9900 . ?
C23B C24B 1.506(17) . ?
C23B C202 1.422(15) . ?
C24A H24A 0.9900 . ?
C24A H24B 0.9900 . ?
C24A C205 1.497(4) . ?
C24B H24C 0.9900 . ?
C24B H24D 0.9900 . ?
C24B C205 1.657(15) . ?
C26A H26A 0.9900 . ?
C26A H26B 0.9900 . ?
C26A C27A 1.532(5) . ?
C26B H26C 0.9900 . ?
C26B H26D 0.9900 . ?
C26B C27B 1.533(17) . ?
C27A H27A 0.9900 . ?
C27A H27B 0.9900 . ?
C27A C208 1.517(4) . ?
C27B H27C 0.9900 . ?
C27B H27D 0.9900 . ?
C27B C208 1.655(15) . ?
C201 H20A 0.9800 . ?
C201 H20B 0.9800 . ?
C201 H20C 0.9800 . ?
C202 H20D 0.9900 . ?
C202 H20E 0.9900 . ?
C202 H20F 0.9900 . ?
C202 H20G 0.9900 . ?
C205 H20H 0.9800 . ?
C205 H20I 0.9800 . ?
C205 H20J 0.9800 . ?
C205 H20K 0.9800 . ?
C205 H20L 0.9800 . ?
C205 H20M 0.9800 . ?
C208 H20N 0.9900 . ?
C208 H20O 0.9900 . ?
C208 H20P 0.9900 . ?
C208 H20Q 0.9900 . ?
C208 C209 1.494(5) . ?
C209 H20R 0.9800 . ?
C209 H20S 0.9800 . ?
C209 H20T 0.9800 . ?
C210 H21E 0.9900 . ?
C210 H21F 0.9900 . ?
C210 H21G 0.9900 . ?
C210 H21H 0.9900 . ?
C301 C302 1.381(4) . ?
C301 C306 1.379(4) . ?
C301 C307 1.512(4) . ?
C302 H302 0.9500 . ?
C302 C303 1.378(4) . ?
C303 H303 0.9500 . ?
C303 C304 1.369(4) . ?
C304 H304 0.9500 . ?
C304 C305 1.378(4) . ?
C305 H305 0.9500 . ?
C305 C306 1.387(4) . ?
C306 H306 0.9500 . ?
C307 H30A 0.9800 . ?
C307 H30B 0.9800 . ?
C307 H30C 0.9800 . ?
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
Ni11 N101 C102 C101 1.4(4) . . . . ?
Ni11 N101 C102 C103 -179.12(18) . . . . ?
Ni11 N101 C105 C104 179.11(18) . . . . ?
Ni11 N101 C105 C106 1.2(4) . . . . ?
Ni11 N102 C107 C106 3.1(4) . . . . ?
Ni11 N102 C107 C108 -178.33(17) . . . . ?
Ni11 N102 C110 C109 177.99(17) . . . . ?
Ni11 N102 C110 C111 -1.6(4) . . . . ?
Ni11 N103 C112 C111 -2.7(4) . . . . ?
Ni11 N103 C112 C113 177.00(18) . . . . ?
Ni11 N103 C115 C114 -177.78(18) . . . . ?
Ni11 N103 C115 C116 0.7(4) . . . . ?
Ni11 N104 C117 C116 1.4(4) . . . . ?
Ni11 N104 C117 C118 -177.48(18) . . . . ?
Ni11 N104 C120 C101 -2.7(4) . . . . ?
Ni11 N104 C120 C119 177.19(18) . . . . ?
N101 C102 C103 C104 0.3(3) . . . . ?
N101 C105 C106 C107 -0.4(4) . . . . ?
N101 C105 C106 C127 179.5(2) . . . . ?
N102 C107 C108 C109 -0.8(3) . . . . ?
N102 C110 C111 C112 2.5(4) . . . . ?
N102 C110 C111 C133 -175.8(2) . . . . ?
N103 C112 C113 C114 1.2(3) . . . . ?
N103 C115 C116 C117 -0.8(4) . . . . ?
N103 C115 C116 C139 178.1(2) . . . . ?
N104 C117 C118 C119 0.1(3) . . . . ?
C101 C102 C103 C104 179.7(3) . . . . ?
C101 C121 C122 C123 179.5(2) . . . . ?
C101 C121 C126 C125 -179.8(3) . . . . ?
C102 N101 C105 C104 0.4(3) . . . . ?
C102 N101 C105 C106 -177.5(3) . . . . ?
C102 C101 C120 N104 0.9(4) . . . . ?
C102 C101 C120 C119 -178.9(3) . . . . ?
C102 C101 C121 C122 75.1(3) . . . . ?
C102 C101 C121 C126 -105.6(3) . . . . ?
C102 C103 C104 C105 0.0(3) . . . . ?
C103 C104 C105 N101 -0.3(3) . . . . ?
C103 C104 C105 C106 177.7(3) . . . . ?
C104 C105 C106 C107 -178.0(3) . . . . ?
C104 C105 C106 C127 1.8(4) . . . . ?
C105 N101 C102 C101 -179.9(3) . . . . ?
C105 N101 C102 C103 -0.4(3) . . . . ?
C105 C106 C107 N102 -1.9(4) . . . . ?
C105 C106 C107 C108 179.7(3) . . . . ?
C105 C106 C127 C128 -113.9(3) . . . . ?
C105 C106 C127 C132 66.7(3) . . . . ?
C106 C107 C108 C109 177.8(3) . . . . ?
C106 C127 C128 C129 179.6(2) . . . . ?
C106 C127 C132 C131 -178.9(2) . . . . ?
C107 N102 C110 C109 -2.1(3) . . . . ?
C107 N102 C110 C111 178.3(3) . . . . ?
C107 C106 C127 C128 66.0(3) . . . . ?
C107 C106 C127 C132 -113.5(3) . . . . ?
C107 C108 C109 C110 -0.5(3) . . . . ?
C108 C109 C110 N102 1.7(3) . . . . ?
C108 C109 C110 C111 -178.7(3) . . . . ?
C109 C110 C111 C112 -177.0(3) . . . . ?
C109 C110 C111 C133 4.7(4) . . . . ?
C110 N102 C107 C106 -176.8(3) . . . . ?
C110 N102 C107 C108 1.8(3) . . . . ?
C110 C111 C112 N103 -0.3(4) . . . . ?
C110 C111 C112 C113 -179.9(3) . . . . ?
C110 C111 C133 C134 -122.5(3) . . . . ?
C110 C111 C133 C138 60.4(4) . . . . ?
C111 C112 C113 C114 -179.1(3) . . . . ?
C111 C133 C134 C135 -175.6(3) . . . . ?
C111 C133 C138 C137 176.8(3) . . . . ?
C112 N103 C115 C114 -0.2(3) . . . . ?
C112 N103 C115 C116 178.3(3) . . . . ?
C112 C111 C133 C134 59.1(4) . . . . ?
C112 C111 C133 C138 -118.0(3) . . . . ?
C112 C113 C114 C115 -1.2(3) . . . . ?
C113 C114 C115 N103 0.9(3) . . . . ?
C113 C114 C115 C116 -177.6(3) . . . . ?
C114 C115 C116 C117 177.5(3) . . . . ?
C114 C115 C116 C139 -3.6(4) . . . . ?
C115 N103 C112 C111 179.7(3) . . . . ?
C115 N103 C112 C113 -0.6(3) . . . . ?
C115 C116 C117 N104 -0.3(4) . . . . ?
C115 C116 C117 C118 178.4(3) . . . . ?
C115 C116 C139 C140 -76.0(3) . . . . ?
C115 C116 C139 C144 104.7(3) . . . . ?
C116 C117 C118 C119 -178.9(3) . . . . ?
C116 C139 C140 C141 -179.5(2) . . . . ?
C116 C139 C144 C143 179.7(2) . . . . ?
C117 N104 C120 C101 179.5(3) . . . . ?
C117 N104 C120 C119 -0.7(3) . . . . ?
C117 C116 C139 C140 103.0(3) . . . . ?
C117 C116 C139 C144 -76.4(3) . . . . ?
C117 C118 C119 C120 -0.5(3) . . . . ?
C118 C119 C120 N104 0.7(3) . . . . ?
C118 C119 C120 C101 -179.4(3) . . . . ?
C120 N104 C117 C116 179.3(3) . . . . ?
C120 N104 C117 C118 0.4(3) . . . . ?
C120 C101 C102 N101 -0.3(4) . . . . ?
C120 C101 C102 C103 -179.7(3) . . . . ?
C120 C101 C121 C122 -104.0(3) . . . . ?
C120 C101 C121 C126 75.4(3) . . . . ?
C121 C101 C102 N101 -179.3(2) . . . . ?
C121 C101 C102 C103 1.3(4) . . . . ?
C121 C101 C120 N104 179.9(2) . . . . ?
C121 C101 C120 C119 0.1(4) . . . . ?
C121 C122 C123 C124 0.8(4) . . . . ?
C122 C121 C126 C125 -0.5(4) . . . . ?
C122 C123 C124 C125 -1.5(4) . . . . ?
C123 C124 C125 C126 1.2(5) . . . . ?
C124 C125 C126 C121 -0.2(4) . . . . ?
C126 C121 C122 C123 0.2(4) . . . . ?
C127 C106 C107 N102 178.3(2) . . . . ?
C127 C106 C107 C108 -0.1(4) . . . . ?
C127 C128 C129 C130 -0.5(4) . . . . ?
C128 C127 C132 C131 1.7(4) . . . . ?
C128 C129 C130 C131 1.3(4) . . . . ?
C129 C130 C131 C132 -0.6(4) . . . . ?
C130 C131 C132 C127 -0.9(4) . . . . ?
C132 C127 C128 C129 -0.9(4) . . . . ?
C133 C111 C112 N103 178.1(2) . . . . ?
C133 C111 C112 C113 -1.6(4) . . . . ?
C133 C134 C135 C136 -1.2(5) . . . . ?
C134 C133 C138 C137 -0.4(4) . . . . ?
C134 C135 C136 C137 -0.4(5) . . . . ?
C135 C136 C137 C138 1.6(5) . . . . ?
C136 C137 C138 C133 -1.2(4) . . . . ?
C138 C133 C134 C135 1.5(4) . . . . ?
C139 C116 C117 N104 -179.2(2) . . . . ?
C139 C116 C117 C118 -0.4(4) . . . . ?
C139 C140 C141 C142 -0.3(4) . . . . ?
C140 C139 C144 C143 0.3(4) . . . . ?
C140 C141 C142 C143 0.5(4) . . . . ?
C141 C142 C143 C144 -0.4(4) . . . . ?
C142 C143 C144 C139 -0.1(4) . . . . ?
C144 C139 C140 C141 -0.1(4) . . . . ?
P21 C26A C27A C208 179.8(3) . . . . ?
P21 C26B C27B C208 172.0(11) . . . . ?
C22A C21A C210 P21 -179.5(4) . . . . ?
C22B C21B C210 P21 -169.8(4) . . . . ?
C24A C23A C202 P21 -165.4(2) . . . . ?
C24B C23B C202 P21 64(2) . . . . ?
C26A P21 C202 C23A -172.0(2) . . . . ?
C26A P21 C210 C21A -150.1(3) . . . . ?
C26A C27A C208 C209 63.6(5) . . . . ?
C26B P21 C202 C23B 130.8(16) . . . . ?
C26B P21 C210 C21B -53.7(7) . . . . ?
C26B C27B C208 C209 176.6(15) . . . . ?
C201 P21 C26A C27A -62.1(3) . . . . ?
C201 P21 C26B C27B -174.9(15) . . . . ?
C201 P21 C202 C23A 67.8(3) . . . . ?
C201 P21 C202 C23B 36.4(14) . . . . ?
C201 P21 C210 C21A -27.7(3) . . . . ?
C201 P21 C210 C21B 34.0(4) . . . . ?
C202 P21 C26A C27A 178.5(3) . . . . ?
C202 P21 C26B C27B 77.1(15) . . . . ?
C202 P21 C210 C21A 93.3(3) . . . . ?
C202 P21 C210 C21B 155.1(3) . . . . ?
C202 C23A C24A C205 -174.5(3) . . . . ?
C202 C23B C24B C205 178.6(13) . . . . ?
C210 P21 C26A C27A 59.9(3) . . . . ?
C210 P21 C26B C27B -66.6(15) . . . . ?
C210 P21 C202 C23A -53.7(3) . . . . ?
C210 P21 C202 C23B -85.1(14) . . . . ?
C210 C21A C22A C1 -65.0(7) . . . . ?
C210 C21B C22B C2 64.8(8) . . . . ?
C301 C302 C303 C304 0.0(5) . . . . ?
C302 C301 C306 C305 0.3(5) . . . . ?
C302 C303 C304 C305 0.8(5) . . . . ?
C303 C304 C305 C306 -1.0(5) . . . . ?
C304 C305 C306 C301 0.5(5) . . . . ?
C306 C301 C302 C303 -0.5(5) . . . . ?
C307 C301 C302 C303 -179.3(3) . . . . ?
C307 C301 C306 C305 179.0(3) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0003 -0.9989 -0.0004 -0.0035 0.0376 0.0150
0.0003 0.9989 0.0004 0.0035 -0.0376 -0.0150
-0.0997 -0.1001 1.0981 0.0308 0.0059 0.0034
0.9990 -0.0008 -1.9976 -0.0334 -0.0206 0.0439
-0.9990 0.0008 1.9976 0.0334 0.0206 -0.0439
-0.0002 0.0001 -0.9992 -0.0309 -0.0001 -0.0070
