#------------------------------------------------------------------------------
#$Date: 2020-10-04 06:06:14 +0300 (Sun, 04 Oct 2020) $
#$Revision: 257050 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/75/4517528.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_4517528
loop_
_publ_author_name
'Bismuto, Alessandro'
'Delcaillau, Tristan'
'Müller, Patrick'
'Morandi, Bill'
_publ_section_title
;
 Nickel-Catalyzed Amination of Aryl Thioethers: A Combined Synthetic and
 Mechanistic Study
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              4630
_journal_page_last               4639
_journal_paper_doi               10.1021/acscatal.0c00393
_journal_year                    2020
_chemical_formula_moiety         'C39 H61 N Ni P2, C3 H3'
_chemical_formula_sum            'C42 H64 N Ni P2'
_chemical_formula_weight         703.59
_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             2019-11-19
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.834(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8848(3)
_cell_length_b                   19.0951(4)
_cell_length_c                   17.6180(4)
_cell_measurement_reflns_used    7158
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      78.5510
_cell_measurement_theta_min      3.8550
_cell_volume                     3846.55(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω     -9.00  27.00   0.50   15.00    --  -49.37  19.00  60.00   72
  2  ω     -9.00  27.00   0.50   15.00    --  -49.37  19.00 120.00   72
  3  ω     -9.00  27.00   0.50   15.00    --  -49.37  19.00 150.00   72
  4  ω     -9.00  27.00   0.50   15.00    --  -49.37  19.00 -90.00   72
  5  ω    -38.00   6.00   0.50   30.00    --  -70.00  38.00 -90.00   88
  6  ω    -68.00   2.00   0.50   30.00    --  -70.00  57.00-120.00  140
  7  ω     59.00 120.00   0.50   15.00    --   48.87 178.00-180.00  122
  8  ω   -120.00 -38.00   0.50   15.00    --  -49.37-178.00  60.00  164
  9  ω   -145.00 -56.00   0.50   30.00    --  -70.00 -38.00 120.00  178
 10  ω     38.00  68.00   0.50   30.00    --  110.00 -57.00 150.00   60
 11  ω     40.00 103.00   0.50   30.00    --  110.00-125.00 150.00  126
 12  ω     38.00  64.00   0.50   30.00    --  110.00 -57.00  30.00   52
 13  ω     40.00  89.00   0.50   30.00    --  110.00 -99.00 -30.00   98
 14  ω     46.00 102.00   0.50   30.00    --  110.00 -99.00 -90.00  112
 15  ω     46.00 117.00   0.50   30.00    --  110.00-125.00-150.00  142
 16  ω     38.00  68.00   0.50   30.00    --  110.00 -57.00-120.00   60
 17  ω     40.00  66.00   0.50   30.00    --  110.00 -57.00 -60.00   52
 18  ω    118.00 176.00   0.50   30.00    --  110.00  19.00-120.00  116
 19  ω    132.00 169.00   0.50   30.00    --  110.00  77.00-150.00   74
 20  ω     99.00 177.00   0.50   30.00    --  110.00  38.00-180.00  156
 21  ω     88.00 114.00   0.50   30.00    --  110.00  77.00-150.00   52
 22  ω    127.00 177.00   0.50   30.00    --  110.00  38.00  30.00  100
 23  ω     40.00  92.00   0.50   30.00    --  110.00-125.00  90.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0036590000
_diffrn_orient_matrix_UB_12      0.0805189000
_diffrn_orient_matrix_UB_13      -0.0063527000
_diffrn_orient_matrix_UB_21      -0.1346978000
_diffrn_orient_matrix_UB_22      -0.0022234000
_diffrn_orient_matrix_UB_23      -0.0246662000
_diffrn_orient_matrix_UB_31      0.0002234000
_diffrn_orient_matrix_UB_32      0.0052394000
_diffrn_orient_matrix_UB_33      0.0872463000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0948
_diffrn_reflns_av_unetI/netI     0.0765
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32151
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.977
_diffrn_reflns_theta_min         3.487
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.717
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.800
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.42a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_description       needle
_exptl_crystal_F_000             1524
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.022
_exptl_crystal_size_min          0.019
_refine_diff_density_max         1.294
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         8081
_refine_ls_number_restraints     159
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0689
_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)+(0.1182P)²+0.4663P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1747
_refine_ls_wR_factor_ref         0.1930
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5751
_reflns_number_total             8081
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cs0c00393_si_007.cif
_cod_data_source_block           bm241019_1_1
_cod_depositor_comments
'Adding full bibliography for 4517528--4517534.cif.'
_cod_original_cell_volume        3846.54(16)
_cod_database_code               4517528
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C45H67NNiP2
_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 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C2A-C1A \\sim C2B-C1B \\sim C3B-C2B \\sim C3A_$1-C1A \\sim C3B_$1-C1B \\sim
C3A-C2A \\sim C3B-C1B_$1
 \\sim C3A_$1-C2A_$1 \\sim C2B_$1-C1B_$1 \\sim C3A-C1A_$1 \\sim C3B_$1-C2B_$1
\\sim C2A_$1-C1A_$1
 with sigma of 0.02
3. Restrained planarity
 C1A_$1, C1A, C2A, C3A_$1, C3A, C2A_$1
 with sigma of 0.1
 C1B_$1, C3B, C2B, C1B, C2B_$1, C3B_$1
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C3B \\sim C2B \\sim C1B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C3A \\sim C1A \\sim C2A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C3B, C2B, C1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3A, C1A, C2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C2, C3, C4, C6, C7, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C3B)=Sof(H3B)=Sof(C2B)=Sof(H2B)=Sof(C1B)=Sof(H1BA)=1-FVAR(1)
 Sof(C1A)=Sof(H1AA)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C16(H16), C22(H22), C28(H28), C34(H34)
7.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B),
 C20(H20A,H20B), C21(H21A,H21B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
  C26(H26A,H26B), C27(H27A,H27B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,
 H31B), C32(H32A,H32B), C33(H33A,H33B), C35(H35A,H35B), C36(H36A,H36B),
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C1A(H1AA), C2A(H2A), C3A(H3A), C3B(H3B), C2B(H2B),
 C1B(H1BA)
7.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_olex2_date_sample_data_collection 2019-10-24
_olex2_date_sample_submission    2019-10-24
_olex2_submission_original_sample_id bm241019_1_1
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.464
_oxdiff_exptl_absorpt_empirical_full_min 0.500
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
Ni1 Ni 0.70121(4) 0.29608(3) 0.33990(3) 0.02445(17) Uani 1 1 d . . . . .
P1 P 0.82917(7) 0.33124(4) 0.28121(5) 0.0240(2) Uani 1 1 d . . . . .
P2 P 0.61005(7) 0.23855(4) 0.22858(5) 0.0262(2) Uani 1 1 d . . . . .
N1 N 0.5803(2) 0.28049(16) 0.39176(17) 0.0326(6) Uani 1 1 d . . . . .
C1 C 0.5149(3) 0.3422(2) 0.4023(2) 0.0431(9) Uani 1 1 d . . . . .
H1A H 0.543695 0.382996 0.379378 0.065 Uiso 1 1 calc R U . . .
H1B H 0.525091 0.350229 0.458682 0.065 Uiso 1 1 calc R U . . .
H1C H 0.431764 0.335193 0.375801 0.065 Uiso 1 1 calc R U . . .
C2 C 0.5607(3) 0.2213(2) 0.4267(2) 0.0362(8) Uani 1 1 d . . . . .
C3 C 0.4627(3) 0.2146(2) 0.4593(2) 0.0432(9) Uani 1 1 d . . . . .
H3 H 0.412382 0.253689 0.457057 0.052 Uiso 1 1 calc R U . . .
C4 C 0.4398(4) 0.1544(2) 0.4931(2) 0.0464(9) Uani 1 1 d . . . . .
H4 H 0.373648 0.151763 0.513413 0.056 Uiso 1 1 calc R U . . .
C5 C 0.5109(4) 0.0979(2) 0.4980(2) 0.0462(9) Uani 1 1 d . . . . .
H5 H 0.494601 0.056122 0.522208 0.055 Uiso 1 1 calc R U . . .
C6 C 0.6080(4) 0.1009(2) 0.4675(3) 0.0503(10) Uani 1 1 d . . . . .
H6 H 0.657333 0.061166 0.471385 0.060 Uiso 1 1 calc R U . . .
C7 C 0.6330(4) 0.1625(2) 0.4313(2) 0.0428(9) Uani 1 1 d . . . . .
H7 H 0.698441 0.164264 0.410130 0.051 Uiso 1 1 calc R U . . .
C8 C 0.8035(3) 0.28708(17) 0.1852(2) 0.0291(7) Uani 1 1 d . . . . .
H8A H 0.829795 0.317975 0.148256 0.035 Uiso 1 1 calc R U . . .
H8B H 0.850706 0.243648 0.191865 0.035 Uiso 1 1 calc R U . . .
C9 C 0.6740(3) 0.26864(16) 0.14956(19) 0.0282(7) Uani 1 1 d . . . . .
H9A H 0.666899 0.231249 0.109599 0.034 Uiso 1 1 calc R U . . .
H9B H 0.631133 0.310319 0.123181 0.034 Uiso 1 1 calc R U . . .
C10 C 0.7858(3) 0.34388(18) 0.4346(2) 0.0303(7) Uani 1 1 d . . . . .
C11 C 0.8525(3) 0.30446(19) 0.4992(2) 0.0332(7) Uani 1 1 d . . . . .
H11 H 0.851790 0.254797 0.495788 0.040 Uiso 1 1 calc R U . . .
C12 C 0.9189(3) 0.3364(2) 0.5673(2) 0.0431(9) Uani 1 1 d . . . . .
H12 H 0.964710 0.308394 0.608935 0.052 Uiso 1 1 calc R U . . .
C13 C 0.9196(4) 0.4084(3) 0.5755(3) 0.0527(11) Uani 1 1 d . . . . .
H13 H 0.966088 0.430082 0.622072 0.063 Uiso 1 1 calc R U . . .
C14 C 0.8510(4) 0.4483(2) 0.5143(3) 0.0502(10) Uani 1 1 d . . . . .
H14 H 0.849064 0.497743 0.519584 0.060 Uiso 1 1 calc R U . . .
C15 C 0.7851(3) 0.4167(2) 0.4455(2) 0.0388(8) Uani 1 1 d . . . . .
H15 H 0.738240 0.445088 0.404767 0.047 Uiso 1 1 calc R U . . .
C16 C 0.9874(3) 0.31565(16) 0.3261(2) 0.0274(7) Uani 1 1 d . . . . .
H16 H 1.027266 0.319734 0.283133 0.033 Uiso 1 1 calc R U . . .
C17 C 1.0041(3) 0.23960(16) 0.3571(2) 0.0301(7) Uani 1 1 d . . . . .
H17A H 0.954267 0.231784 0.393140 0.036 Uiso 1 1 calc R U . . .
H17B H 0.977879 0.206935 0.312112 0.036 Uiso 1 1 calc R U . . .
C18 C 1.1309(3) 0.22329(18) 0.4008(2) 0.0345(8) Uani 1 1 d . . . . .
H18A H 1.136402 0.175282 0.422749 0.041 Uiso 1 1 calc R U . . .
H18B H 1.180020 0.225612 0.363644 0.041 Uiso 1 1 calc R U . . .
C19 C 1.1754(3) 0.27567(19) 0.4673(2) 0.0360(8) Uani 1 1 d . . . . .
H19A H 1.257023 0.264133 0.496370 0.043 Uiso 1 1 calc R U . . .
H19B H 1.126780 0.273120 0.504773 0.043 Uiso 1 1 calc R U . . .
C20 C 1.1702(3) 0.34955(18) 0.4334(2) 0.0350(8) Uani 1 1 d . . . . .
H20A H 1.219395 0.352012 0.396306 0.042 Uiso 1 1 calc R U . . .
H20B H 1.201633 0.383305 0.476653 0.042 Uiso 1 1 calc R U . . .
C21 C 1.0444(3) 0.36935(16) 0.3903(2) 0.0299(7) Uani 1 1 d . . . . .
H21A H 1.043818 0.416016 0.365698 0.036 Uiso 1 1 calc R U . . .
H21B H 0.997720 0.372539 0.428914 0.036 Uiso 1 1 calc R U . . .
C22 C 0.8174(3) 0.42591(16) 0.2587(2) 0.0286(7) Uani 1 1 d . . . . .
H22 H 0.845655 0.450899 0.310257 0.034 Uiso 1 1 calc R U . . .
C23 C 0.8918(3) 0.45253(19) 0.2062(2) 0.0358(8) Uani 1 1 d . . . . .
H23A H 0.866489 0.429378 0.154031 0.043 Uiso 1 1 calc R U . . .
H23B H 0.974817 0.440292 0.230444 0.043 Uiso 1 1 calc R U . . .
C24 C 0.8802(3) 0.5320(2) 0.1954(3) 0.0430(9) Uani 1 1 d . . . . .
H24A H 0.912690 0.555270 0.246973 0.052 Uiso 1 1 calc R U . . .
H24B H 0.925882 0.547631 0.159252 0.052 Uiso 1 1 calc R U . . .
C25 C 0.7528(3) 0.55335(19) 0.1620(2) 0.0417(9) Uani 1 1 d . . . . .
H25A H 0.747310 0.605055 0.158969 0.050 Uiso 1 1 calc R U . . .
H25B H 0.722976 0.534525 0.107867 0.050 Uiso 1 1 calc R U . . .
C26 C 0.6776(3) 0.52622(18) 0.2129(2) 0.0385(8) Uani 1 1 d . . . . .
H26A H 0.594780 0.538287 0.187832 0.046 Uiso 1 1 calc R U . . .
H26B H 0.701472 0.549399 0.265114 0.046 Uiso 1 1 calc R U . . .
C27 C 0.6890(3) 0.44736(16) 0.2240(2) 0.0305(7) Uani 1 1 d . . . . .
H27A H 0.657172 0.423870 0.172504 0.037 Uiso 1 1 calc R U . . .
H27B H 0.642565 0.431876 0.259842 0.037 Uiso 1 1 calc R U . . .
C28 C 0.4511(3) 0.25443(17) 0.1878(2) 0.0298(7) Uani 1 1 d . . . . .
H28 H 0.428526 0.238607 0.131551 0.036 Uiso 1 1 calc R U . . .
C29 C 0.4217(3) 0.33278(18) 0.1887(2) 0.0318(7) Uani 1 1 d . . . . .
H29A H 0.447552 0.350412 0.243612 0.038 Uiso 1 1 calc R U . . .
H29B H 0.464904 0.358945 0.157083 0.038 Uiso 1 1 calc R U . . .
C30 C 0.2900(3) 0.3461(2) 0.1553(2) 0.0376(8) Uani 1 1 d . . . . .
H30A H 0.273746 0.396454 0.160485 0.045 Uiso 1 1 calc R U . . .
H30B H 0.266310 0.334218 0.098408 0.045 Uiso 1 1 calc R U . . .
C31 C 0.2177(3) 0.3027(2) 0.1979(2) 0.0436(9) Uani 1 1 d . . . . .
H31A H 0.233329 0.319001 0.253154 0.052 Uiso 1 1 calc R U . . .
H31B H 0.133423 0.309607 0.171803 0.052 Uiso 1 1 calc R U . . .
C32 C 0.2474(3) 0.2257(2) 0.1970(2) 0.0386(8) Uani 1 1 d . . . . .
H32A H 0.223267 0.208320 0.141978 0.046 Uiso 1 1 calc R U . . .
H32B H 0.202994 0.199234 0.227620 0.046 Uiso 1 1 calc R U . . .
C33 C 0.3776(3) 0.21227(19) 0.2318(2) 0.0340(8) Uani 1 1 d . . . . .
H33A H 0.393765 0.161687 0.228316 0.041 Uiso 1 1 calc R U . . .
H33B H 0.400528 0.225640 0.288240 0.041 Uiso 1 1 calc R U . . .
C34 C 0.6213(3) 0.14138(17) 0.2274(2) 0.0321(7) Uani 1 1 d . . . . .
H34 H 0.582452 0.123340 0.267209 0.039 Uiso 1 1 calc R U . . .
C35 C 0.5584(4) 0.10712(19) 0.1481(2) 0.0457(10) Uani 1 1 d . . . . .
H35A H 0.475513 0.122062 0.132150 0.055 Uiso 1 1 calc R U . . .
H35B H 0.595285 0.122797 0.106949 0.055 Uiso 1 1 calc R U . . .
C36 C 0.5648(4) 0.0272(2) 0.1547(3) 0.0513(11) Uani 1 1 d . . . . .
H36A H 0.520090 0.011214 0.191311 0.062 Uiso 1 1 calc R U . . .
H36B H 0.528667 0.006246 0.102290 0.062 Uiso 1 1 calc R U . . .
C37 C 0.6916(4) 0.0022(2) 0.1847(3) 0.0563(12) Uani 1 1 d . . . . .
H37A H 0.692600 -0.049232 0.191769 0.068 Uiso 1 1 calc R U . . .
H37B H 0.733700 0.013143 0.144765 0.068 Uiso 1 1 calc R U . . .
C38 C 0.7543(4) 0.03664(19) 0.2623(3) 0.0489(10) Uani 1 1 d . . . . .
H38A H 0.836895 0.021101 0.278529 0.059 Uiso 1 1 calc R U . . .
H38B H 0.717098 0.022120 0.303715 0.059 Uiso 1 1 calc R U . . .
C39 C 0.7494(3) 0.11684(18) 0.2542(3) 0.0404(9) Uani 1 1 d . . . . .
H39A H 0.790741 0.131682 0.215097 0.049 Uiso 1 1 calc R U . . .
H39B H 0.789096 0.138622 0.305499 0.049 Uiso 1 1 calc R U . . .
C1A C 0.1163(4) 0.4836(3) 0.0224(3) 0.0501(15) Uani 0.821(9) 1 d D U P A 1
H1AA H 0.197234 0.472333 0.038150 0.060 Uiso 0.821(9) 1 calc R U P A 1
C2A C 0.0821(4) 0.5519(3) 0.0032(3) 0.0438(13) Uani 0.821(9) 1 d D U P A 1
H2A H 0.139132 0.587286 0.005297 0.053 Uiso 0.821(9) 1 calc R U P A 1
C3A C -0.0345(6) 0.5685(3) -0.0189(3) 0.0395(15) Uani 0.821(9) 1 d D U P A 1
H3A H -0.058913 0.615466 -0.031702 0.047 Uiso 0.821(9) 1 calc R U P A 1
C3B C -0.0529(19) 0.5265(11) -0.0715(19) 0.059(8) Uani 0.179(9) 1 d D U P A 2
H3B H -0.090840 0.544159 -0.122432 0.071 Uiso 0.179(9) 1 calc R U P A 2
C2B C -0.003(3) 0.5736(19) -0.0126(18) 0.069(11) Uani 0.179(9) 1 d D U P A 2
H2B H -0.005863 0.622661 -0.021679 0.083 Uiso 0.179(9) 1 calc R U P A 2
C1B C 0.050(2) 0.5454(11) 0.060(2) 0.063(8) Uani 0.179(9) 1 d D U P A 2
H1BA H 0.085400 0.575413 0.103041 0.075 Uiso 0.179(9) 1 calc R U 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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
1 2 0 0.0108
-1 -2 0 0.0099
0 -1 0 0.0081
0 1 0 0.0135
0 0 1 0.0786
2 -3 -11 0.0803
-1 2 0 0.0126
-2 1 0 0.0117
-7 4 3 0.0234
1 0 0 0.0063
-7 0 -1 0.0126
-7 -4 5 0.0363
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
P1 Ni1 P2 88.22(4) . . ?
N1 Ni1 P1 170.74(10) . . ?
N1 Ni1 P2 95.39(9) . . ?
N1 Ni1 C10 86.72(13) . . ?
C10 Ni1 P1 89.90(11) . . ?
C10 Ni1 P2 177.46(11) . . ?
C8 P1 Ni1 109.58(11) . . ?
C8 P1 C16 102.30(15) . . ?
C8 P1 C22 105.48(16) . . ?
C16 P1 Ni1 120.59(12) . . ?
C22 P1 Ni1 112.59(12) . . ?
C22 P1 C16 104.90(14) . . ?
C9 P2 Ni1 107.76(10) . . ?
C9 P2 C28 104.01(15) . . ?
C9 P2 C34 104.82(16) . . ?
C28 P2 Ni1 117.08(11) . . ?
C28 P2 C34 103.15(15) . . ?
C34 P2 Ni1 118.51(11) . . ?
C1 N1 Ni1 115.5(3) . . ?
C2 N1 Ni1 126.5(3) . . ?
C2 N1 C1 117.5(3) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 121.3(4) . . ?
N1 C2 C7 121.4(4) . . ?
C7 C2 C3 117.2(4) . . ?
C2 C3 H3 118.9 . . ?
C4 C3 C2 122.1(4) . . ?
C4 C3 H3 118.9 . . ?
C3 C4 H4 119.8 . . ?
C3 C4 C5 120.3(4) . . ?
C5 C4 H4 119.8 . . ?
C4 C5 H5 119.8 . . ?
C4 C5 C6 120.5(4) . . ?
C6 C5 H5 119.8 . . ?
C5 C6 H6 119.8 . . ?
C5 C6 C7 120.4(4) . . ?
C7 C6 H6 119.8 . . ?
C2 C7 C6 119.5(4) . . ?
C2 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
P1 C8 H8A 109.2 . . ?
P1 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
C9 C8 P1 112.2(2) . . ?
C9 C8 H8A 109.2 . . ?
C9 C8 H8B 109.2 . . ?
P2 C9 H9A 109.8 . . ?
P2 C9 H9B 109.8 . . ?
C8 C9 P2 109.6(2) . . ?
C8 C9 H9A 109.8 . . ?
C8 C9 H9B 109.8 . . ?
H9A C9 H9B 108.2 . . ?
C11 C10 Ni1 119.4(3) . . ?
C15 C10 Ni1 124.6(3) . . ?
C15 C10 C11 116.1(3) . . ?
C10 C11 H11 119.2 . . ?
C12 C11 C10 121.7(3) . . ?
C12 C11 H11 119.2 . . ?
C11 C12 H12 119.5 . . ?
C13 C12 C11 121.0(4) . . ?
C13 C12 H12 119.5 . . ?
C12 C13 H13 120.7 . . ?
C12 C13 C14 118.6(4) . . ?
C14 C13 H13 120.7 . . ?
C13 C14 H14 119.6 . . ?
C15 C14 C13 120.7(4) . . ?
C15 C14 H14 119.6 . . ?
C10 C15 H15 119.1 . . ?
C14 C15 C10 121.8(4) . . ?
C14 C15 H15 119.1 . . ?
P1 C16 H16 107.4 . . ?
C17 C16 P1 108.6(2) . . ?
C17 C16 H16 107.4 . . ?
C21 C16 P1 113.5(2) . . ?
C21 C16 H16 107.4 . . ?
C21 C16 C17 112.2(3) . . ?
C16 C17 H17A 109.1 . . ?
C16 C17 H17B 109.1 . . ?
H17A C17 H17B 107.8 . . ?
C18 C17 C16 112.6(3) . . ?
C18 C17 H17A 109.1 . . ?
C18 C17 H17B 109.1 . . ?
C17 C18 H18A 109.7 . . ?
C17 C18 H18B 109.7 . . ?
H18A C18 H18B 108.2 . . ?
C19 C18 C17 110.0(3) . . ?
C19 C18 H18A 109.7 . . ?
C19 C18 H18B 109.7 . . ?
C18 C19 H19A 109.7 . . ?
C18 C19 H19B 109.7 . . ?
C18 C19 C20 109.7(3) . . ?
H19A C19 H19B 108.2 . . ?
C20 C19 H19A 109.7 . . ?
C20 C19 H19B 109.7 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 C21 110.7(3) . . ?
H20A C20 H20B 108.1 . . ?
C21 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
C16 C21 H21A 109.2 . . ?
C16 C21 H21B 109.2 . . ?
C20 C21 C16 112.0(3) . . ?
C20 C21 H21A 109.2 . . ?
C20 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
P1 C22 H22 106.5 . . ?
C23 C22 P1 115.6(2) . . ?
C23 C22 H22 106.5 . . ?
C23 C22 C27 110.3(3) . . ?
C27 C22 P1 110.8(2) . . ?
C27 C22 H22 106.5 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 C24 110.9(3) . . ?
H23A C23 H23B 108.0 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
C23 C24 H24A 109.4 . . ?
C23 C24 H24B 109.4 . . ?
H24A C24 H24B 108.0 . . ?
C25 C24 C23 111.1(3) . . ?
C25 C24 H24A 109.4 . . ?
C25 C24 H24B 109.4 . . ?
C24 C25 H25A 109.4 . . ?
C24 C25 H25B 109.4 . . ?
H25A C25 H25B 108.0 . . ?
C26 C25 C24 111.3(3) . . ?
C26 C25 H25A 109.4 . . ?
C26 C25 H25B 109.4 . . ?
C25 C26 H26A 109.3 . . ?
C25 C26 H26B 109.3 . . ?
C25 C26 C27 111.6(3) . . ?
H26A C26 H26B 108.0 . . ?
C27 C26 H26A 109.3 . . ?
C27 C26 H26B 109.3 . . ?
C22 C27 H27A 109.4 . . ?
C22 C27 H27B 109.4 . . ?
C26 C27 C22 111.0(3) . . ?
C26 C27 H27A 109.4 . . ?
C26 C27 H27B 109.4 . . ?
H27A C27 H27B 108.0 . . ?
P2 C28 H28 107.7 . . ?
C29 C28 P2 111.4(2) . . ?
C29 C28 H28 107.7 . . ?
C29 C28 C33 109.9(3) . . ?
C33 C28 P2 112.1(2) . . ?
C33 C28 H28 107.7 . . ?
C28 C29 H29A 109.3 . . ?
C28 C29 H29B 109.3 . . ?
H29A C29 H29B 108.0 . . ?
C30 C29 C28 111.6(3) . . ?
C30 C29 H29A 109.3 . . ?
C30 C29 H29B 109.3 . . ?
C29 C30 H30A 109.2 . . ?
C29 C30 H30B 109.2 . . ?
H30A C30 H30B 107.9 . . ?
C31 C30 C29 111.8(3) . . ?
C31 C30 H30A 109.2 . . ?
C31 C30 H30B 109.2 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 108.0 . . ?
C32 C31 C30 110.9(3) . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
C31 C32 H32A 109.2 . . ?
C31 C32 H32B 109.2 . . ?
C31 C32 C33 111.9(3) . . ?
H32A C32 H32B 107.9 . . ?
C33 C32 H32A 109.2 . . ?
C33 C32 H32B 109.2 . . ?
C28 C33 H33A 109.4 . . ?
C28 C33 H33B 109.4 . . ?
C32 C33 C28 111.2(3) . . ?
C32 C33 H33A 109.4 . . ?
C32 C33 H33B 109.4 . . ?
H33A C33 H33B 108.0 . . ?
P2 C34 H34 106.7 . . ?
C35 C34 P2 114.5(2) . . ?
C35 C34 H34 106.7 . . ?
C39 C34 P2 111.6(2) . . ?
C39 C34 H34 106.7 . . ?
C39 C34 C35 110.1(3) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 108.1 . . ?
C36 C35 C34 110.7(3) . . ?
C36 C35 H35A 109.5 . . ?
C36 C35 H35B 109.5 . . ?
C35 C36 H36A 109.4 . . ?
C35 C36 H36B 109.4 . . ?
H36A C36 H36B 108.0 . . ?
C37 C36 C35 111.2(4) . . ?
C37 C36 H36A 109.4 . . ?
C37 C36 H36B 109.4 . . ?
C36 C37 H37A 109.3 . . ?
C36 C37 H37B 109.3 . . ?
H37A C37 H37B 107.9 . . ?
C38 C37 C36 111.8(3) . . ?
C38 C37 H37A 109.3 . . ?
C38 C37 H37B 109.3 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 C39 110.5(4) . . ?
H38A C38 H38B 108.1 . . ?
C39 C38 H38A 109.5 . . ?
C39 C38 H38B 109.5 . . ?
C34 C39 H39A 109.7 . . ?
C34 C39 H39B 109.7 . . ?
C38 C39 C34 109.9(3) . . ?
C38 C39 H39A 109.7 . . ?
C38 C39 H39B 109.7 . . ?
H39A C39 H39B 108.2 . . ?
C2A C1A H1AA 119.5 . . ?
C2A C1A C3A 120.9(5) . 3_565 ?
C3A C1A H1AA 119.5 3_565 . ?
C1A C2A H2A 120.2 . . ?
C3A C2A C1A 119.7(5) . . ?
C3A C2A H2A 120.2 . . ?
C1A C3A H3A 120.3 3_565 . ?
C2A C3A C1A 119.4(5) . 3_565 ?
C2A C3A H3A 120.3 . . ?
C2B C3B H3B 118.3 . . ?
C1B C3B H3B 118.3 3_565 . ?
C3B C2B H2B 122.0 . . ?
C1B C2B C3B 116(3) . . ?
C1B C2B H2B 122.0 . . ?
C3B C1B H1BA 119.7 3_565 . ?
C2B C1B H1BA 119.7 . . ?
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 P1 2.1658(10) . ?
Ni1 P2 2.2511(9) . ?
Ni1 N1 1.925(3) . ?
Ni1 C10 1.926(3) . ?
P1 C8 1.840(3) . ?
P1 C16 1.854(3) . ?
P1 C22 1.848(3) . ?
P2 C9 1.850(4) . ?
P2 C28 1.853(3) . ?
P2 C34 1.861(3) . ?
N1 C1 1.452(5) . ?
N1 C2 1.338(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.438(6) . ?
C2 C7 1.402(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.356(6) . ?
C4 H4 0.9500 . ?
C4 C5 1.359(6) . ?
C5 H5 0.9500 . ?
C5 C6 1.400(7) . ?
C6 H6 0.9500 . ?
C6 C7 1.408(6) . ?
C7 H7 0.9500 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.536(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.414(5) . ?
C10 C15 1.403(5) . ?
C11 H11 0.9500 . ?
C11 C12 1.385(5) . ?
C12 H12 0.9500 . ?
C12 C13 1.382(6) . ?
C13 H13 0.9500 . ?
C13 C14 1.389(7) . ?
C14 H14 0.9500 . ?
C14 C15 1.389(6) . ?
C15 H15 0.9500 . ?
C16 H16 1.0000 . ?
C16 C17 1.545(4) . ?
C16 C21 1.540(4) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.526(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.521(5) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.527(5) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.529(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22 1.0000 . ?
C22 C23 1.530(5) . ?
C22 C27 1.537(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.530(5) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.523(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.519(6) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.520(4) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28 1.0000 . ?
C28 C29 1.538(5) . ?
C28 C33 1.543(5) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.536(5) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.530(6) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.514(6) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.523(5) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34 1.0000 . ?
C34 C35 1.539(5) . ?
C34 C39 1.539(5) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.531(5) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C37 1.530(7) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.518(7) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.538(5) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C1A H1AA 0.9500 . ?
C1A C2A 1.381(6) . ?
C1A C3A 1.381(7) 3_565 ?
C2A H2A 0.9500 . ?
C2A C3A 1.371(7) . ?
C3A H3A 0.9500 . ?
C3B H3B 0.9500 . ?
C3B C2B 1.378(12) . ?
C3B C1B 1.385(11) 3_565 ?
C2B H2B 0.9500 . ?
C2B C1B 1.375(12) . ?
C1B H1BA 0.9500 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 P1 C8 C9 29.7(2) . . . . ?
Ni1 P1 C16 C17 44.3(3) . . . . ?
Ni1 P1 C16 C21 -81.2(2) . . . . ?
Ni1 P1 C22 C23 -171.0(2) . . . . ?
Ni1 P1 C22 C27 -44.6(3) . . . . ?
Ni1 P2 C9 C8 32.0(2) . . . . ?
Ni1 P2 C28 C29 44.2(3) . . . . ?
Ni1 P2 C28 C33 -79.5(2) . . . . ?
Ni1 P2 C34 C35 -178.6(3) . . . . ?
Ni1 P2 C34 C39 -52.7(3) . . . . ?
Ni1 N1 C2 C3 -176.1(2) . . . . ?
Ni1 N1 C2 C7 2.4(5) . . . . ?
Ni1 C10 C11 C12 177.1(3) . . . . ?
Ni1 C10 C15 C14 -177.9(3) . . . . ?
P1 C8 C9 P2 -39.1(3) . . . . ?
P1 C16 C17 C18 -175.7(2) . . . . ?
P1 C16 C21 C20 172.5(2) . . . . ?
P1 C22 C23 C24 -176.8(2) . . . . ?
P1 C22 C27 C26 174.4(3) . . . . ?
P2 C28 C29 C30 -179.8(3) . . . . ?
P2 C28 C33 C32 -179.6(3) . . . . ?
P2 C34 C35 C36 -175.8(3) . . . . ?
P2 C34 C39 C38 173.0(3) . . . . ?
N1 C2 C3 C4 178.3(3) . . . . ?
N1 C2 C7 C6 -179.1(3) . . . . ?
C1 N1 C2 C3 12.6(5) . . . . ?
C1 N1 C2 C7 -169.0(3) . . . . ?
C2 C3 C4 C5 0.8(6) . . . . ?
C3 C2 C7 C6 -0.6(5) . . . . ?
C3 C4 C5 C6 -0.6(6) . . . . ?
C4 C5 C6 C7 -0.2(6) . . . . ?
C5 C6 C7 C2 0.7(6) . . . . ?
C7 C2 C3 C4 -0.2(5) . . . . ?
C8 P1 C16 C17 -77.5(3) . . . . ?
C8 P1 C16 C21 157.0(2) . . . . ?
C8 P1 C22 C23 -51.5(3) . . . . ?
C8 P1 C22 C27 74.9(3) . . . . ?
C9 P2 C28 C29 -74.5(3) . . . . ?
C9 P2 C28 C33 161.8(2) . . . . ?
C9 P2 C34 C35 -58.5(3) . . . . ?
C9 P2 C34 C39 67.5(3) . . . . ?
C10 C11 C12 C13 2.0(6) . . . . ?
C11 C10 C15 C14 3.2(6) . . . . ?
C11 C12 C13 C14 0.8(7) . . . . ?
C12 C13 C14 C15 -1.5(7) . . . . ?
C13 C14 C15 C10 -0.6(7) . . . . ?
C15 C10 C11 C12 -3.8(5) . . . . ?
C16 P1 C8 C9 158.8(2) . . . . ?
C16 P1 C22 C23 56.1(3) . . . . ?
C16 P1 C22 C27 -177.5(2) . . . . ?
C16 C17 C18 C19 55.4(4) . . . . ?
C17 C16 C21 C20 48.9(4) . . . . ?
C17 C18 C19 C20 -60.9(4) . . . . ?
C18 C19 C20 C21 61.0(4) . . . . ?
C19 C20 C21 C16 -55.0(4) . . . . ?
C21 C16 C17 C18 -49.5(4) . . . . ?
C22 P1 C8 C9 -91.7(2) . . . . ?
C22 P1 C16 C17 172.6(2) . . . . ?
C22 P1 C16 C21 47.1(3) . . . . ?
C22 C23 C24 C25 -56.3(4) . . . . ?
C23 C22 C27 C26 -56.3(4) . . . . ?
C23 C24 C25 C26 55.4(5) . . . . ?
C24 C25 C26 C27 -55.3(4) . . . . ?
C25 C26 C27 C22 55.9(4) . . . . ?
C27 C22 C23 C24 56.5(4) . . . . ?
C28 P2 C9 C8 157.0(2) . . . . ?
C28 P2 C34 C35 50.1(3) . . . . ?
C28 P2 C34 C39 176.1(3) . . . . ?
C28 C29 C30 C31 54.7(4) . . . . ?
C29 C28 C33 C32 55.9(4) . . . . ?
C29 C30 C31 C32 -54.3(4) . . . . ?
C30 C31 C32 C33 55.6(4) . . . . ?
C31 C32 C33 C28 -57.0(4) . . . . ?
C33 C28 C29 C30 -54.9(4) . . . . ?
C34 P2 C9 C8 -95.1(2) . . . . ?
C34 P2 C28 C29 176.3(3) . . . . ?
C34 P2 C28 C33 52.6(3) . . . . ?
C34 C35 C36 C37 -55.3(5) . . . . ?
C35 C34 C39 C38 -58.7(4) . . . . ?
C35 C36 C37 C38 55.1(5) . . . . ?
C36 C37 C38 C39 -56.4(5) . . . . ?
C37 C38 C39 C34 58.1(5) . . . . ?
C39 C34 C35 C36 57.5(5) . . . . ?
C1A C2A C3A C1A -0.6(9) . . . 3_565 ?
C3A C1A C2A C3A 0.6(9) 3_565 . . . ?
C3B C2B C1B C3B 0.3(16) . . . 3_565 ?
C1B C3B C2B C1B -0.3(17) 3_565 . . . ?
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
1.0000 2.0000 -0.0000 0.1574 -0.1391 0.0107
-1.0000 -2.0000 0.0000 -0.1574 0.1391 -0.0107
0.0000 -1.0000 -0.0000 -0.0805 0.0022 -0.0052
-0.0000 1.0000 0.0000 0.0805 -0.0022 0.0052
0.0000 0.0000 1.0000 -0.0064 -0.0247 0.0872
2.3361 -2.9277 -11.1110 -0.1737 -0.0341 -0.9842
-1.0000 2.0000 0.0001 0.1647 0.1303 0.0103
-2.0000 1.0000 0.0001 0.0878 0.2672 0.0048
-7.3312 3.8737 2.7761 0.3211 0.9104 0.2609
1.0000 0.0000 -0.0000 -0.0037 -0.1347 0.0002
-7.2320 -0.0835 -0.8969 0.0254 0.9964 -0.0803
-7.1109 -4.3452 4.7329 -0.3539 0.8507 0.3886
