#------------------------------------------------------------------------------
#$Date: 2020-07-06 05:57:55 +0300 (Mon, 06 Jul 2020) $
#$Revision: 253868 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/45/7704524.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_7704524
loop_
_publ_author_name
'Burt, Liam K.'
'Hill, Anthony F.'
_publ_section_title
;
 Heterobimetallic μ₂-carbido complexes of platinum and
 tungsten.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8143
_journal_page_last               8161
_journal_paper_doi               10.1039/d0dt01617a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C44 H46 B Br N6 O2 P2 Pt W, 2(C2 H3 N)'
_chemical_formula_sum            'C48 H52 B Br N8 O2 P2 Pt W'
_chemical_formula_weight         1304.57
_chemical_properties_physical
Air-sensitive,Heat-sensitive,Oxygen-sensitive,Light-sensitive,Photo-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-04-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-04-18 deposited with the CCDC.	2020-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.0110(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.18910(10)
_cell_length_b                   10.52850(10)
_cell_length_c                   19.67920(10)
_cell_measurement_reflns_used    45224
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.6030
_cell_measurement_theta_min      4.7100
_cell_volume                     2401.73(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -104.00 -20.00   1.00    1.15    --  -36.95 -57.00-180.00   84
  2  ω      5.00  31.00   1.00    1.15    --   36.95  86.00 -81.97   26
  3  ω      6.00  76.00   1.00    1.15    --   36.95 -99.00   0.00   70
  4  ω      3.00  29.00   1.00    1.15    --   36.95  90.00-171.38   26
  5  ω    -32.00 106.00   1.00    1.15    --   36.95   0.00   0.00  138
  6  ω     10.00  42.00   1.00    1.15    --   36.95  78.00 -54.12   32
  7  ω     18.00 106.00   1.00    1.15    --   36.95  38.00 150.00   88
  8  ω     20.00 104.00   1.00    1.15    --   36.95  57.00-180.00   84
  9  ω     20.00 104.00   1.00    1.15    --   36.95  57.00 -30.00   84
 10  ω    -21.00  64.00   1.00    1.15    --   36.95 -77.00   0.00   85
 11  ω     27.00  90.00   1.00    1.15    --   36.95-125.00  90.00   63
 12  ω     41.00 136.00   1.00    4.61    --  111.00 -25.00  90.00   95
 13  ω     42.00 106.00   1.00    4.61    --  111.00 -92.00   0.00   64
 14  ω     86.00 178.00   1.00    4.61    --  111.00  25.00 -30.00   92
 15  ω     41.00 109.00   1.00    4.61    --  111.00-111.00-180.00   68
 16  ω     41.00 109.00   1.00    4.61    --  111.00-111.00  60.00   68
 17  ω     41.00 109.00   1.00    4.61    --  111.00-111.00  90.00   68
 18  ω     41.00 109.00   1.00    4.61    --  111.00-111.00-150.00   68
 19  ω     61.00 146.00   1.00    4.61    --  111.00 178.00-180.00   85
 20  ω     61.00 146.00   1.00    4.61    --  111.00 178.00 -30.00   85
 21  ω     42.00 106.00   1.00    4.61    --  111.00 -92.00-180.00   64
 22  ω     44.00 131.00   1.00    4.61    --  111.00 -64.00-120.00   87
 23  ω     61.00 146.00   1.00    4.61    --  111.00 178.00   0.00   85
 24  ω     91.00 178.00   1.00    4.61    --  111.00  64.00 -90.00   87
 25  ω     92.00 178.00   1.00    4.61    --  111.00  38.00   0.00   86
 26  ω     41.00 109.00   1.00    4.61    --  111.00-111.00 -30.00   68
 27  ω     43.00 138.00   1.00    4.61    --  111.00 -77.00  90.00   95
 28  ω     65.00 178.00   1.00    4.61    --  111.00  12.00 -60.00  113
 29  ω     42.00 130.00   1.00    4.61    --  111.00 -38.00 150.00   88
 30  ω     44.00 131.00   1.00    4.61    --  111.00 -64.00  90.00   87
 31  ω     41.00 157.00   1.00    4.61    --  111.00 -12.00  90.00  116
 32  ω     43.00 138.00   1.00    4.61    --  111.00 -77.00-150.00   95
 33  ω     42.00 130.00   1.00    4.61    --  111.00 -38.00  90.00   88
 34  ω     41.00 109.00   1.00    4.61    --  111.00-111.00 -90.00   68
 35  ω     43.00 138.00   1.00    4.61    --  111.00 -77.00  30.00   95
 36  ω     41.00 157.00   1.00    4.61    --  111.00 -12.00 -30.00  116
 37  ω     41.00 109.00   1.00    4.61    --  111.00-111.00  30.00   68
 38  ω     42.00 106.00   1.00    4.61    --  111.00 -92.00  90.00   64
 39  ω     41.00 109.00   1.00    4.61    --  111.00-111.00 150.00   68
 40  ω     41.00 109.00   1.00    4.61    --  111.00-111.00 120.00   68
 41  ω     42.00 106.00   1.00    4.61    --  111.00 -92.00 -30.00   64
 42  ω     43.00 128.00   1.00    4.61    --  111.00 -50.00 -60.00   85
 43  ω     92.00 178.00   1.00    4.61    --  111.00  38.00 120.00   86
 44  ω     43.00 138.00   1.00    4.61    --  111.00 -77.00 -60.00   95
 45  ω     42.00 130.00   1.00    4.61    --  111.00 -38.00 -60.00   88
 46  ω     42.00 130.00   1.00    4.61    --  111.00 -38.00-150.00   88
 47  ω     41.00 109.00   1.00    4.61    --  111.00-111.00-120.00   68
 48  ω    103.00 178.00   1.00    4.61    --  111.00  77.00-120.00   75
 49  ω     42.00 106.00   1.00    4.61    --  111.00 -92.00  30.00   64
 50  ω     44.00 131.00   1.00    4.61    --  111.00 -64.00 -90.00   87
 51  ω     40.00 139.00   1.00    4.61    --  111.00 -21.00 -51.35   99
 52  ω    -21.00  64.00   1.00    1.15    --   36.95 -77.00-120.00   85
 53  ω      4.00  30.00   1.00    1.15    --   36.95  89.00  64.31   26
 54  ω    -30.00  54.00   1.00    1.15    --   36.95 -57.00-180.00   84
 55  ω      4.00  30.00   1.00    1.15    --   36.95  88.00  -5.20   26
 56  ω      5.00  31.00   1.00    1.15    --   36.95  87.00 106.37   26
 57  ω    -32.00  56.00   1.00    1.15    --   36.95 -38.00-120.00   88
 58  ω    -32.00  56.00   1.00    1.15    --   36.95 -38.00  90.00   88
 59  ω     20.00 104.00   1.00    1.15    --   36.95  57.00  90.00   84
 60  ω     20.00 104.00   1.00    1.15    --   36.95  57.00 150.00   84
 61  ω     18.00 106.00   1.00    1.15    --   36.95  38.00  60.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0847443000
_diffrn_orient_matrix_UB_12      -0.0692532000
_diffrn_orient_matrix_UB_13      -0.0638030000
_diffrn_orient_matrix_UB_21      -0.0050620000
_diffrn_orient_matrix_UB_22      -0.1124668000
_diffrn_orient_matrix_UB_23      0.0490292000
_diffrn_orient_matrix_UB_31      -0.1022313000
_diffrn_orient_matrix_UB_32      0.0630410000
_diffrn_orient_matrix_UB_33      0.0173594000
_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  0.0439
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            56214
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.909
_diffrn_reflns_theta_min         3.813
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.712
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.36a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.804
_exptl_crystal_description       needle
_exptl_crystal_F_000             1268
_exptl_crystal_preparation
'Vap. Diff. Et2O into MeCN @ 0 degrees celcius'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.038
_refine_diff_density_max         1.131
_refine_diff_density_min         -1.111
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
 Flack x determined using 4370 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.034(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         9573
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0271
_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)+(0.0558P)²+1.7696P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0733
_reflns_Friedel_coverage         0.865
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.967
_reflns_number_gt                9520
_reflns_number_total             9573
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt01617a2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7704524--7704531.cif.'
_cod_database_code               7704524
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C96 H104 B2 Br2 N16 O4 P4 Pt2 W2'
_chemical_oxdiff_usercomment     'Vap diff. Et2O in MeCN'
_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 99.07
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B1-H1
 1.15 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C11(H11), C16(H16), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
 C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C51(H51), C52(H52), C53(H53),
  C54(H54), C55(H55), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C18(H18A,H18B,H18C), C67(H67A,H67B,H67C), C69(H69A,H69B,
 H69C)
;
_ins_header
;
TITL LB008_2_scale in P2(1) 
REM P2(1) (#4 in standard setting)
CELL 1.54184  12.189082  10.528521  19.679215  90.0000 108.0114  90.0000
ZERR    2.00   0.000068   0.000051   0.000133   0.0000   0.0007   0.0000
LATT -1
SYMM -x, y+1/2,-z 
SFAC C H B N O P Br W Pt
UNIT 192.00 208.00 4.00 32.00 8.00 8.00 4.00 4.00 4.00
TREF
HKLF 4
END
;
_olex2_submission_original_sample_id LB008
_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 1.590
_oxdiff_exptl_absorpt_empirical_full_min 0.723
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
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
Pt1 Pt 0.67653(2) 0.42450(2) 0.36643(2) 0.01598(8) Uani 1 1 d . . . . .
W1 W 0.43083(2) 0.33535(3) 0.19950(2) 0.01585(8) Uani 1 1 d . . . . .
Br1 Br 0.69743(7) 0.19483(8) 0.39416(4) 0.02944(16) Uani 1 1 d . . . . .
P1 P 0.84046(13) 0.47490(16) 0.46093(9) 0.0171(3) Uani 1 1 d . . . . .
P2 P 0.66541(14) 0.63194(15) 0.34380(9) 0.0171(3) Uani 1 1 d . . . . .
O1 O 0.3110(6) 0.2310(6) 0.3073(4) 0.0414(15) Uani 1 1 d . . . . .
O2 O 0.5517(6) 0.0699(6) 0.2288(3) 0.0344(12) Uani 1 1 d . . . . .
N1 N 0.2909(5) 0.2585(6) 0.0980(3) 0.0223(12) Uani 1 1 d . . . . .
N2 N 0.2512(5) 0.3347(6) 0.0383(3) 0.0192(10) Uani 1 1 d . . . . .
N3 N 0.5047(5) 0.3938(5) 0.1140(3) 0.0192(10) Uani 1 1 d . . . . .
N4 N 0.4385(5) 0.4528(5) 0.0524(3) 0.0193(11) Uani 1 1 d . . . . .
N5 N 0.3217(4) 0.5101(5) 0.1659(3) 0.0170(10) Uani 1 1 d . . . . .
N6 N 0.2841(5) 0.5494(6) 0.0953(3) 0.0192(11) Uani 1 1 d . . . . .
C1 C 0.5439(6) 0.3882(6) 0.2798(3) 0.0159(11) Uani 1 1 d . . . . .
C2 C 0.3524(7) 0.2717(7) 0.2677(4) 0.0265(14) Uani 1 1 d . . . . .
C3 C 0.5104(6) 0.1676(7) 0.2178(3) 0.0241(14) Uani 1 1 d . . . . .
C4 C 0.2387(7) 0.0472(8) 0.1361(5) 0.0347(17) Uani 1 1 d . . . . .
H4A H 0.249442 -0.031218 0.114101 0.052 Uiso 1 1 calc R U . . .
H4B H 0.171043 0.041238 0.151150 0.052 Uiso 1 1 calc R U . . .
H4C H 0.304768 0.063456 0.176835 0.052 Uiso 1 1 calc R U . . .
C5 C 0.2241(6) 0.1537(7) 0.0833(4) 0.0256(14) Uani 1 1 d . . . . .
C6 C 0.1440(6) 0.1640(8) 0.0154(4) 0.0293(16) Uani 1 1 d . . . . .
H6 H 0.088882 0.104073 -0.007439 0.035 Uiso 1 1 calc R U . . .
C7 C 0.1624(6) 0.2787(8) -0.0109(4) 0.0276(15) Uani 1 1 d . . . . .
C8 C 0.0980(7) 0.3423(10) -0.0802(4) 0.0360(16) Uani 1 1 d . . . . .
H8A H 0.061357 0.417935 -0.070537 0.054 Uiso 1 1 calc R U . . .
H8B H 0.040447 0.285402 -0.108697 0.054 Uiso 1 1 calc R U . . .
H8C H 0.150956 0.364248 -0.105679 0.054 Uiso 1 1 calc R U . . .
C9 C 0.7101(6) 0.3317(8) 0.1682(4) 0.0302(15) Uani 1 1 d . . . . .
H9A H 0.712091 0.367412 0.213446 0.045 Uiso 1 1 calc R U . . .
H9B H 0.781553 0.349226 0.159094 0.045 Uiso 1 1 calc R U . . .
H9C H 0.699160 0.241480 0.169154 0.045 Uiso 1 1 calc R U . . .
C10 C 0.6125(6) 0.3893(7) 0.1103(4) 0.0247(14) Uani 1 1 d . . . . .
C11 C 0.6154(6) 0.4459(7) 0.0463(4) 0.0279(15) Uani 1 1 d . . . . .
H11 H 0.679343 0.454022 0.030397 0.033 Uiso 1 1 calc R U . . .
C12 C 0.5060(6) 0.4865(7) 0.0120(4) 0.0255(14) Uani 1 1 d . . . . .
C13 C 0.4617(8) 0.5620(9) -0.0552(4) 0.0339(16) Uani 1 1 d . . . . .
H13A H 0.405013 0.513177 -0.090196 0.051 Uiso 1 1 calc R U . . .
H13B H 0.524433 0.582205 -0.073153 0.051 Uiso 1 1 calc R U . . .
H13C H 0.427250 0.639070 -0.045468 0.051 Uiso 1 1 calc R U . . .
C14 C 0.3027(6) 0.5821(7) 0.2814(4) 0.0267(15) Uani 1 1 d . . . . .
H14A H 0.238701 0.539133 0.289930 0.040 Uiso 1 1 calc R U . . .
H14B H 0.310848 0.665057 0.302649 0.040 Uiso 1 1 calc R U . . .
H14C H 0.371975 0.534200 0.302183 0.040 Uiso 1 1 calc R U . . .
C15 C 0.2818(5) 0.5943(6) 0.2034(4) 0.0194(12) Uani 1 1 d . . . . .
C16 C 0.2200(6) 0.6894(7) 0.1576(4) 0.0251(13) Uani 1 1 d . . . . .
H16 H 0.183946 0.759444 0.170077 0.030 Uiso 1 1 calc R U . . .
C17 C 0.2235(6) 0.6579(7) 0.0901(4) 0.0239(13) Uani 1 1 d . . . . .
C18 C 0.1725(7) 0.7246(8) 0.0202(4) 0.0309(16) Uani 1 1 d . . . . .
H18A H 0.233294 0.756554 0.003465 0.046 Uiso 1 1 calc R U . . .
H18B H 0.125413 0.794026 0.026461 0.046 Uiso 1 1 calc R U . . .
H18C H 0.125973 0.666111 -0.014204 0.046 Uiso 1 1 calc R U . . .
C20 C 0.8453(6) 0.6483(7) 0.4671(4) 0.0218(13) Uani 1 1 d . . . . .
H20A H 0.794162 0.678135 0.492894 0.026 Uiso 1 1 calc R U . . .
H20B H 0.923045 0.676404 0.492396 0.026 Uiso 1 1 calc R U . . .
C21 C 0.8073(6) 0.7011(7) 0.3912(4) 0.0224(13) Uani 1 1 d . . . . .
H21A H 0.862856 0.678574 0.366986 0.027 Uiso 1 1 calc R U . . .
H21B H 0.801765 0.792907 0.392178 0.027 Uiso 1 1 calc R U . . .
C30 C 0.8616(5) 0.4193(7) 0.5516(3) 0.0202(12) Uani 1 1 d . . . . .
C31 C 0.8418(7) 0.4970(8) 0.6042(4) 0.0305(15) Uani 1 1 d . . . . .
H31 H 0.818931 0.580865 0.593730 0.037 Uiso 1 1 calc R U . . .
C32 C 0.8562(8) 0.4487(9) 0.6722(4) 0.0366(19) Uani 1 1 d . . . . .
H32 H 0.842685 0.500510 0.707063 0.044 Uiso 1 1 calc R U . . .
C33 C 0.8902(7) 0.3254(9) 0.6881(4) 0.0329(16) Uani 1 1 d . . . . .
H33 H 0.901963 0.294671 0.734083 0.039 Uiso 1 1 calc R U . . .
C34 C 0.9071(7) 0.2460(8) 0.6358(4) 0.0313(15) Uani 1 1 d . . . . .
H34 H 0.927703 0.161525 0.646274 0.038 Uiso 1 1 calc R U . . .
C35 C 0.8931(6) 0.2938(7) 0.5677(4) 0.0236(13) Uani 1 1 d . . . . .
H35 H 0.904874 0.240992 0.532763 0.028 Uiso 1 1 calc R U . . .
C40 C 0.9732(6) 0.4347(7) 0.4424(3) 0.0205(12) Uani 1 1 d . . . . .
C41 C 1.0804(6) 0.4733(7) 0.4886(4) 0.0222(13) Uani 1 1 d . . . . .
H41 H 1.084144 0.515200 0.530858 0.027 Uiso 1 1 calc R U . . .
C42 C 1.1809(6) 0.4495(7) 0.4720(4) 0.0281(16) Uani 1 1 d . . . . .
H42 H 1.251413 0.476532 0.502759 0.034 Uiso 1 1 calc R U . . .
C43 C 1.1771(7) 0.3857(7) 0.4097(4) 0.0296(16) Uani 1 1 d . . . . .
H43 H 1.244854 0.369213 0.399029 0.036 Uiso 1 1 calc R U . . .
C44 C 1.0721(7) 0.3466(8) 0.3635(4) 0.0301(14) Uani 1 1 d . . . . .
H44 H 1.069659 0.303773 0.321747 0.036 Uiso 1 1 calc R U . . .
C45 C 0.9696(6) 0.3710(7) 0.3791(4) 0.0257(14) Uani 1 1 d . . . . .
H45 H 0.899228 0.345124 0.347609 0.031 Uiso 1 1 calc R U . . .
C50 C 0.5701(6) 0.7186(7) 0.3826(4) 0.0221(13) Uani 1 1 d . . . . .
C51 C 0.5509(6) 0.8491(8) 0.3706(4) 0.0289(14) Uani 1 1 d . . . . .
H51 H 0.583266 0.891899 0.340095 0.035 Uiso 1 1 calc R U . . .
C52 C 0.4840(7) 0.9135(9) 0.4040(5) 0.0390(18) Uani 1 1 d . . . . .
H52 H 0.468871 0.999478 0.394815 0.047 Uiso 1 1 calc R U . . .
C53 C 0.4384(7) 0.8501(11) 0.4517(5) 0.042(2) Uani 1 1 d . . . . .
H53 H 0.394058 0.894054 0.474756 0.051 Uiso 1 1 calc R U . . .
C54 C 0.4595(7) 0.7225(10) 0.4645(4) 0.0379(19) Uani 1 1 d . . . . .
H54 H 0.430314 0.680883 0.496854 0.045 Uiso 1 1 calc R U . . .
C55 C 0.5240(7) 0.6555(8) 0.4293(4) 0.0298(15) Uani 1 1 d . . . . .
H55 H 0.536183 0.568825 0.437150 0.036 Uiso 1 1 calc R U . . .
C60 C 0.6366(6) 0.6812(6) 0.2520(3) 0.0203(12) Uani 1 1 d . . . . .
C61 C 0.5331(6) 0.7356(8) 0.2119(4) 0.0265(14) Uani 1 1 d . . . . .
H61 H 0.475238 0.750832 0.232589 0.032 Uiso 1 1 calc R U . . .
C62 C 0.5160(7) 0.7672(8) 0.1406(4) 0.0328(17) Uani 1 1 d . . . . .
H62 H 0.446753 0.803804 0.113683 0.039 Uiso 1 1 calc R U . . .
C63 C 0.6015(8) 0.7442(8) 0.1099(4) 0.0346(17) Uani 1 1 d . . . . .
H63 H 0.590241 0.766942 0.062594 0.042 Uiso 1 1 calc R U . . .
C64 C 0.7045(8) 0.6874(8) 0.1491(4) 0.0341(17) Uani 1 1 d . . . . .
H64 H 0.760863 0.669596 0.127674 0.041 Uiso 1 1 calc R U . . .
C65 C 0.7227(7) 0.6576(7) 0.2200(4) 0.0266(14) Uani 1 1 d . . . . .
H65 H 0.792335 0.621646 0.246736 0.032 Uiso 1 1 calc R U . . .
B1 B 0.3083(6) 0.4661(7) 0.0370(4) 0.0202(14) Uani 1 1 d D . . . .
H1 H 0.261(7) 0.515(9) -0.016(3) 0.024 Uiso 1 1 d D U . . .
N7 N 0.9754(8) 0.5572(10) 0.2039(6) 0.055(2) Uani 1 1 d . . . . .
C66 C 1.0092(7) 0.4772(9) 0.1758(5) 0.0350(17) Uani 1 1 d . . . . .
C67 C 1.0527(9) 0.3775(10) 0.1415(6) 0.051(2) Uani 1 1 d . . . . .
H67A H 1.052387 0.405170 0.095016 0.076 Uiso 1 1 calc R U . . .
H67B H 1.004592 0.303724 0.136927 0.076 Uiso 1 1 calc R U . . .
H67C H 1.130051 0.356828 0.169758 0.076 Uiso 1 1 calc R U . . .
N8 N 1.0635(10) 0.6113(13) 0.8076(7) 0.071(3) Uani 1 1 d . . . . .
C68 C 1.1088(9) 0.5636(11) 0.7723(7) 0.051(2) Uani 1 1 d . . . . .
C69 C 1.1671(10) 0.4997(13) 0.7285(7) 0.060(3) Uani 1 1 d . . . . .
H69A H 1.112220 0.451202 0.692286 0.089 Uiso 1 1 calc R U . . .
H69B H 1.224881 0.444008 0.757763 0.089 Uiso 1 1 calc R U . . .
H69C H 1.202909 0.561487 0.706353 0.089 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 0.0181 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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 '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'
O O 0.0492 0.0322 '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'
Pt Pt -4.5932 6.9264 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 '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
-7 1 8 0.0536
7 0 -8 0.0329
1 -7 3 0.0872
-1 7 -3 0.1012
0 0 12 0.0228
1 0 -12 0.0134
-7 3 2 0.0582
7 -3 0 0.0593
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 Pt1 Br1 92.41(5) . . ?
P2 Pt1 Br1 177.66(5) . . ?
P2 Pt1 P1 85.44(6) . . ?
C1 Pt1 Br1 90.13(18) . . ?
C1 Pt1 P1 174.76(19) . . ?
C1 Pt1 P2 91.94(19) . . ?
N3 W1 N1 79.0(2) . . ?
N3 W1 N5 83.79(19) . . ?
N5 W1 N1 79.8(2) . . ?
C1 W1 N1 177.3(3) . . ?
C1 W1 N3 101.3(2) . . ?
C1 W1 N5 103.0(2) . . ?
C1 W1 C2 84.8(3) . . ?
C1 W1 C3 85.4(3) . . ?
C2 W1 N1 94.8(2) . . ?
C2 W1 N3 173.7(3) . . ?
C2 W1 N5 96.4(2) . . ?
C2 W1 C3 83.6(3) . . ?
C3 W1 N1 91.9(3) . . ?
C3 W1 N3 95.4(2) . . ?
C3 W1 N5 171.6(2) . . ?
C20 P1 Pt1 106.4(2) . . ?
C30 P1 Pt1 122.4(2) . . ?
C30 P1 C20 105.3(3) . . ?
C40 P1 Pt1 112.6(2) . . ?
C40 P1 C20 103.5(3) . . ?
C40 P1 C30 104.9(3) . . ?
C21 P2 Pt1 107.3(2) . . ?
C50 P2 Pt1 114.5(2) . . ?
C50 P2 C21 102.2(3) . . ?
C60 P2 Pt1 117.6(2) . . ?
C60 P2 C21 104.7(3) . . ?
C60 P2 C50 108.9(3) . . ?
N2 N1 W1 119.9(5) . . ?
C5 N1 W1 134.5(5) . . ?
C5 N1 N2 105.3(6) . . ?
N1 N2 B1 119.4(5) . . ?
C7 N2 N1 110.5(6) . . ?
C7 N2 B1 130.1(6) . . ?
N4 N3 W1 121.7(4) . . ?
C10 N3 W1 131.6(5) . . ?
C10 N3 N4 106.7(5) . . ?
N3 N4 B1 120.3(5) . . ?
C12 N4 N3 109.7(5) . . ?
C12 N4 B1 129.9(6) . . ?
N6 N5 W1 121.5(4) . . ?
C15 N5 W1 131.5(4) . . ?
C15 N5 N6 107.0(5) . . ?
N5 N6 B1 119.7(5) . . ?
C17 N6 N5 109.5(6) . . ?
C17 N6 B1 130.7(6) . . ?
W1 C1 Pt1 172.7(4) . . ?
O1 C2 W1 177.0(7) . . ?
O2 C3 W1 177.1(7) . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
C5 C4 H4C 109.5 . . ?
N1 C5 C4 121.9(7) . . ?
N1 C5 C6 109.9(7) . . ?
C6 C5 C4 128.2(7) . . ?
C5 C6 H6 126.7 . . ?
C7 C6 C5 106.5(7) . . ?
C7 C6 H6 126.7 . . ?
N2 C7 C6 107.8(7) . . ?
N2 C7 C8 122.4(7) . . ?
C6 C7 C8 129.7(7) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C10 C9 H9A 109.5 . . ?
C10 C9 H9B 109.5 . . ?
C10 C9 H9C 109.5 . . ?
N3 C10 C9 122.4(6) . . ?
N3 C10 C11 109.3(7) . . ?
C11 C10 C9 128.3(6) . . ?
C10 C11 H11 126.7 . . ?
C12 C11 C10 106.6(6) . . ?
C12 C11 H11 126.7 . . ?
N4 C12 C11 107.8(6) . . ?
N4 C12 C13 122.7(7) . . ?
C11 C12 C13 129.4(7) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
C15 C14 H14C 109.5 . . ?
N5 C15 C14 122.6(6) . . ?
N5 C15 C16 109.4(6) . . ?
C16 C15 C14 127.9(6) . . ?
C15 C16 H16 126.9 . . ?
C17 C16 C15 106.1(6) . . ?
C17 C16 H16 126.9 . . ?
N6 C17 C16 108.0(6) . . ?
N6 C17 C18 122.0(7) . . ?
C16 C17 C18 130.0(7) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
P1 C20 H20A 110.2 . . ?
P1 C20 H20B 110.2 . . ?
H20A C20 H20B 108.5 . . ?
C21 C20 P1 107.7(5) . . ?
C21 C20 H20A 110.2 . . ?
C21 C20 H20B 110.2 . . ?
P2 C21 H21A 110.1 . . ?
P2 C21 H21B 110.1 . . ?
C20 C21 P2 107.8(5) . . ?
C20 C21 H21A 110.1 . . ?
C20 C21 H21B 110.1 . . ?
H21A C21 H21B 108.5 . . ?
C31 C30 P1 122.2(6) . . ?
C35 C30 P1 118.5(5) . . ?
C35 C30 C31 119.2(6) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 C30 120.0(8) . . ?
C32 C31 H31 120.0 . . ?
C31 C32 H32 119.8 . . ?
C33 C32 C31 120.3(7) . . ?
C33 C32 H32 119.8 . . ?
C32 C33 H33 119.8 . . ?
C32 C33 C34 120.4(7) . . ?
C34 C33 H33 119.8 . . ?
C33 C34 H34 120.2 . . ?
C33 C34 C35 119.5(8) . . ?
C35 C34 H34 120.2 . . ?
C30 C35 C34 120.6(7) . . ?
C30 C35 H35 119.7 . . ?
C34 C35 H35 119.7 . . ?
C41 C40 P1 120.8(5) . . ?
C41 C40 C45 118.8(6) . . ?
C45 C40 P1 120.3(5) . . ?
C40 C41 H41 119.7 . . ?
C42 C41 C40 120.6(7) . . ?
C42 C41 H41 119.7 . . ?
C41 C42 H42 119.8 . . ?
C43 C42 C41 120.4(7) . . ?
C43 C42 H42 119.8 . . ?
C42 C43 H43 120.1 . . ?
C44 C43 C42 119.8(7) . . ?
C44 C43 H43 120.1 . . ?
C43 C44 H44 119.7 . . ?
C43 C44 C45 120.5(7) . . ?
C45 C44 H44 119.7 . . ?
C40 C45 H45 120.1 . . ?
C44 C45 C40 119.8(7) . . ?
C44 C45 H45 120.1 . . ?
C51 C50 P2 121.0(6) . . ?
C55 C50 P2 118.7(6) . . ?
C55 C50 C51 120.1(7) . . ?
C50 C51 H51 120.1 . . ?
C52 C51 C50 119.7(8) . . ?
C52 C51 H51 120.1 . . ?
C51 C52 H52 119.9 . . ?
C51 C52 C53 120.2(9) . . ?
C53 C52 H52 119.9 . . ?
C52 C53 H53 120.1 . . ?
C54 C53 C52 119.9(8) . . ?
C54 C53 H53 120.1 . . ?
C53 C54 H54 119.8 . . ?
C53 C54 C55 120.5(8) . . ?
C55 C54 H54 119.8 . . ?
C50 C55 C54 119.7(8) . . ?
C50 C55 H55 120.2 . . ?
C54 C55 H55 120.2 . . ?
C61 C60 P2 123.3(5) . . ?
C61 C60 C65 119.5(6) . . ?
C65 C60 P2 117.2(5) . . ?
C60 C61 H61 120.1 . . ?
C60 C61 C62 119.8(7) . . ?
C62 C61 H61 120.1 . . ?
C61 C62 H62 120.0 . . ?
C63 C62 C61 120.1(8) . . ?
C63 C62 H62 120.0 . . ?
C62 C63 H63 119.7 . . ?
C62 C63 C64 120.6(7) . . ?
C64 C63 H63 119.7 . . ?
C63 C64 H64 120.2 . . ?
C65 C64 C63 119.6(7) . . ?
C65 C64 H64 120.2 . . ?
C60 C65 H65 119.8 . . ?
C64 C65 C60 120.4(7) . . ?
C64 C65 H65 119.8 . . ?
N2 B1 H1 109(5) . . ?
N4 B1 N2 111.0(5) . . ?
N4 B1 N6 109.3(5) . . ?
N4 B1 H1 115(4) . . ?
N6 B1 N2 107.8(5) . . ?
N6 B1 H1 105(5) . . ?
N7 C66 C67 179.3(12) . . ?
C66 C67 H67A 109.5 . . ?
C66 C67 H67B 109.5 . . ?
C66 C67 H67C 109.5 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
N8 C68 C69 178.4(15) . . ?
C68 C69 H69A 109.5 . . ?
C68 C69 H69B 109.5 . . ?
C68 C69 H69C 109.5 . . ?
H69A C69 H69B 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 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
Pt1 Br1 2.4747(8) . ?
Pt1 P1 2.3312(16) . ?
Pt1 P2 2.2248(16) . ?
Pt1 C1 1.990(7) . ?
W1 N1 2.334(6) . ?
W1 N3 2.227(5) . ?
W1 N5 2.247(5) . ?
W1 C1 1.833(7) . ?
W1 C2 1.990(8) . ?
W1 C3 1.993(8) . ?
P1 C20 1.830(7) . ?
P1 C30 1.819(7) . ?
P1 C40 1.815(7) . ?
P2 C21 1.841(7) . ?
P2 C50 1.820(7) . ?
P2 C60 1.806(7) . ?
O1 C2 1.134(10) . ?
O2 C3 1.136(10) . ?
N1 N2 1.381(8) . ?
N1 C5 1.348(10) . ?
N2 C7 1.345(9) . ?
N2 B1 1.553(9) . ?
N3 N4 1.378(8) . ?
N3 C10 1.339(9) . ?
N4 C12 1.355(8) . ?
N4 B1 1.528(9) . ?
N5 N6 1.383(8) . ?
N5 C15 1.339(8) . ?
N6 C17 1.347(9) . ?
N6 B1 1.543(9) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C4 C5 1.502(11) . ?
C5 C6 1.394(11) . ?
C6 H6 0.9300 . ?
C6 C7 1.359(12) . ?
C7 C8 1.505(11) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C9 C10 1.497(10) . ?
C10 C11 1.403(11) . ?
C11 H11 0.9300 . ?
C11 C12 1.364(11) . ?
C12 C13 1.494(10) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C14 C15 1.482(9) . ?
C15 C16 1.400(10) . ?
C16 H16 0.9300 . ?
C16 C17 1.382(10) . ?
C17 C18 1.499(10) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C21 1.526(9) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C30 C31 1.398(10) . ?
C30 C35 1.385(11) . ?
C31 H31 0.9300 . ?
C31 C32 1.391(11) . ?
C32 H32 0.9300 . ?
C32 C33 1.369(14) . ?
C33 H33 0.9300 . ?
C33 C34 1.390(12) . ?
C34 H34 0.9300 . ?
C34 C35 1.391(10) . ?
C35 H35 0.9300 . ?
C40 C41 1.402(9) . ?
C40 C45 1.403(9) . ?
C41 H41 0.9300 . ?
C41 C42 1.385(10) . ?
C42 H42 0.9300 . ?
C42 C43 1.385(11) . ?
C43 H43 0.9300 . ?
C43 C44 1.383(12) . ?
C44 H44 0.9300 . ?
C44 C45 1.400(10) . ?
C45 H45 0.9300 . ?
C50 C51 1.402(11) . ?
C50 C55 1.386(10) . ?
C51 H51 0.9300 . ?
C51 C52 1.374(11) . ?
C52 H52 0.9300 . ?
C52 C53 1.400(14) . ?
C53 H53 0.9300 . ?
C53 C54 1.375(15) . ?
C54 H54 0.9300 . ?
C54 C55 1.389(11) . ?
C55 H55 0.9300 . ?
C60 C61 1.388(10) . ?
C60 C65 1.403(10) . ?
C61 H61 0.9300 . ?
C61 C62 1.394(10) . ?
C62 H62 0.9300 . ?
C62 C63 1.378(13) . ?
C63 H63 0.9300 . ?
C63 C64 1.388(13) . ?
C64 H64 0.9300 . ?
C64 C65 1.380(11) . ?
C65 H65 0.9300 . ?
B1 H1 1.15(3) . ?
N7 C66 1.151(13) . ?
C66 C67 1.435(13) . ?
C67 H67A 0.9600 . ?
C67 H67B 0.9600 . ?
C67 H67C 0.9600 . ?
N8 C68 1.131(17) . ?
C68 C69 1.441(17) . ?
C69 H69A 0.9600 . ?
C69 H69B 0.9600 . ?
C69 H69C 0.9600 . ?
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
Pt1 P1 C20 C21 -39.0(5) . . . . ?
Pt1 P1 C30 C31 -101.0(6) . . . . ?
Pt1 P1 C30 C35 75.8(5) . . . . ?
Pt1 P1 C40 C41 171.4(5) . . . . ?
Pt1 P1 C40 C45 -4.8(6) . . . . ?
Pt1 P2 C21 C20 -46.5(5) . . . . ?
Pt1 P2 C50 C51 -177.5(5) . . . . ?
Pt1 P2 C50 C55 7.9(7) . . . . ?
Pt1 P2 C60 C61 110.0(6) . . . . ?
Pt1 P2 C60 C65 -67.4(6) . . . . ?
W1 N1 N2 C7 -173.0(4) . . . . ?
W1 N1 N2 B1 5.5(7) . . . . ?
W1 N1 C5 C4 -6.6(11) . . . . ?
W1 N1 C5 C6 172.4(5) . . . . ?
W1 N3 N4 C12 175.5(4) . . . . ?
W1 N3 N4 B1 -7.1(8) . . . . ?
W1 N3 C10 C9 3.5(11) . . . . ?
W1 N3 C10 C11 -176.1(5) . . . . ?
W1 N5 N6 C17 -178.2(4) . . . . ?
W1 N5 N6 B1 5.3(7) . . . . ?
W1 N5 C15 C14 -2.1(10) . . . . ?
W1 N5 C15 C16 178.2(5) . . . . ?
P1 C20 C21 P2 54.5(5) . . . . ?
P1 C30 C31 C32 178.2(6) . . . . ?
P1 C30 C35 C34 -178.2(6) . . . . ?
P1 C40 C41 C42 -175.9(6) . . . . ?
P1 C40 C45 C44 176.6(6) . . . . ?
P2 C50 C51 C52 -176.1(6) . . . . ?
P2 C50 C55 C54 174.3(6) . . . . ?
P2 C60 C61 C62 -177.8(6) . . . . ?
P2 C60 C65 C64 177.1(6) . . . . ?
N1 N2 C7 C6 -1.1(8) . . . . ?
N1 N2 C7 C8 177.1(6) . . . . ?
N1 N2 B1 N4 55.0(7) . . . . ?
N1 N2 B1 N6 -64.7(7) . . . . ?
N1 C5 C6 C7 -0.8(9) . . . . ?
N2 N1 C5 C4 -178.9(7) . . . . ?
N2 N1 C5 C6 0.1(8) . . . . ?
N3 N4 C12 C11 1.9(8) . . . . ?
N3 N4 C12 C13 -174.8(7) . . . . ?
N3 N4 B1 N2 -55.8(8) . . . . ?
N3 N4 B1 N6 63.0(7) . . . . ?
N3 C10 C11 C12 1.0(9) . . . . ?
N4 N3 C10 C9 179.8(6) . . . . ?
N4 N3 C10 C11 0.2(8) . . . . ?
N5 N6 C17 C16 -0.7(8) . . . . ?
N5 N6 C17 C18 179.3(6) . . . . ?
N5 N6 B1 N2 59.3(7) . . . . ?
N5 N6 B1 N4 -61.5(7) . . . . ?
N5 C15 C16 C17 0.5(8) . . . . ?
N6 N5 C15 C14 178.6(6) . . . . ?
N6 N5 C15 C16 -1.0(7) . . . . ?
C4 C5 C6 C7 178.1(7) . . . . ?
C5 N1 N2 C7 0.6(7) . . . . ?
C5 N1 N2 B1 179.2(6) . . . . ?
C5 C6 C7 N2 1.1(8) . . . . ?
C5 C6 C7 C8 -176.9(8) . . . . ?
C7 N2 B1 N4 -126.7(7) . . . . ?
C7 N2 B1 N6 113.6(7) . . . . ?
C9 C10 C11 C12 -178.7(7) . . . . ?
C10 N3 N4 C12 -1.3(7) . . . . ?
C10 N3 N4 B1 176.1(6) . . . . ?
C10 C11 C12 N4 -1.7(8) . . . . ?
C10 C11 C12 C13 174.6(8) . . . . ?
C12 N4 B1 N2 121.0(7) . . . . ?
C12 N4 B1 N6 -120.2(7) . . . . ?
C14 C15 C16 C17 -179.1(7) . . . . ?
C15 N5 N6 C17 1.1(7) . . . . ?
C15 N5 N6 B1 -175.4(6) . . . . ?
C15 C16 C17 N6 0.1(8) . . . . ?
C15 C16 C17 C18 -180.0(7) . . . . ?
C17 N6 B1 N2 -116.3(7) . . . . ?
C17 N6 B1 N4 122.9(7) . . . . ?
C20 P1 C30 C31 20.4(6) . . . . ?
C20 P1 C30 C35 -162.8(5) . . . . ?
C20 P1 C40 C41 56.9(6) . . . . ?
C20 P1 C40 C45 -119.2(6) . . . . ?
C21 P2 C50 C51 66.9(6) . . . . ?
C21 P2 C50 C55 -107.8(6) . . . . ?
C21 P2 C60 C61 -131.1(6) . . . . ?
C21 P2 C60 C65 51.6(6) . . . . ?
C30 P1 C20 C21 -170.3(4) . . . . ?
C30 P1 C40 C41 -53.3(7) . . . . ?
C30 P1 C40 C45 130.6(6) . . . . ?
C30 C31 C32 C33 0.2(12) . . . . ?
C31 C30 C35 C34 -1.3(10) . . . . ?
C31 C32 C33 C34 -2.0(12) . . . . ?
C32 C33 C34 C35 2.1(12) . . . . ?
C33 C34 C35 C30 -0.4(11) . . . . ?
C35 C30 C31 C32 1.4(11) . . . . ?
C40 P1 C20 C21 79.9(5) . . . . ?
C40 P1 C30 C31 129.2(6) . . . . ?
C40 P1 C30 C35 -54.0(6) . . . . ?
C40 C41 C42 C43 -0.8(11) . . . . ?
C41 C40 C45 C44 0.4(11) . . . . ?
C41 C42 C43 C44 0.7(11) . . . . ?
C42 C43 C44 C45 0.0(12) . . . . ?
C43 C44 C45 C40 -0.5(12) . . . . ?
C45 C40 C41 C42 0.3(11) . . . . ?
C50 P2 C21 C20 74.2(5) . . . . ?
C50 P2 C60 C61 -22.4(7) . . . . ?
C50 P2 C60 C65 160.3(6) . . . . ?
C50 C51 C52 C53 2.2(12) . . . . ?
C51 C50 C55 C54 -0.4(11) . . . . ?
C51 C52 C53 C54 -0.9(13) . . . . ?
C52 C53 C54 C55 -1.1(13) . . . . ?
C53 C54 C55 C50 1.8(13) . . . . ?
C55 C50 C51 C52 -1.5(11) . . . . ?
C60 P2 C21 C20 -172.2(5) . . . . ?
C60 P2 C50 C51 -43.5(7) . . . . ?
C60 P2 C50 C55 141.8(6) . . . . ?
C60 C61 C62 C63 0.2(12) . . . . ?
C61 C60 C65 C64 -0.4(11) . . . . ?
C61 C62 C63 C64 1.2(13) . . . . ?
C62 C63 C64 C65 -2.1(13) . . . . ?
C63 C64 C65 C60 1.7(12) . . . . ?
C65 C60 C61 C62 -0.6(11) . . . . ?
B1 N2 C7 C6 -179.5(6) . . . . ?
B1 N2 C7 C8 -1.3(11) . . . . ?
B1 N4 C12 C11 -175.2(7) . . . . ?
B1 N4 C12 C13 8.2(12) . . . . ?
B1 N6 C17 C16 175.2(6) . . . . ?
B1 N6 C17 C18 -4.7(11) . . . . ?
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
-7.3829 1.1633 7.5389 0.0641 0.2762 0.9590
7.3485 0.0460 -8.1773 -0.1042 -0.4433 -0.8903
1.0082 -6.5556 2.5493 0.2059 0.8572 -0.4721
-0.9295 6.5570 -2.6375 -0.2070 -0.8621 0.4626
-0.2926 0.1318 12.2838 -0.7681 0.5889 0.2515
0.5291 -0.2314 -12.3783 0.7610 -0.5836 -0.2836
-7.0628 2.9722 2.0919 0.2592 -0.1960 0.9457
6.7616 -2.8437 0.3964 -0.4014 0.3050 -0.8636
