#------------------------------------------------------------------------------
#$Date: 2020-06-05 12:49:08 +0300 (Fri, 05 Jun 2020) $
#$Revision: 252701 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/64/7126402.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_7126402
loop_
_publ_author_name
'Burt, Liam K.'
'Cordiner, Richard L.'
'Hill, Anthony F.'
'Manzano, Richard A.'
'Wagler, Jörg'
_publ_section_title
;
 The significance of phosphoniocarbynes in halocarbyne cross-coupling
 reactions.
;
_journal_issue                   42
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5673
_journal_page_last               5676
_journal_paper_doi               10.1039/d0cc02070b
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C54 H52 B Br N6 O2 P2 Pd W'
_chemical_formula_sum            'C52 H52 B Br N6 O2 P2 Pd W'
_chemical_formula_weight         1235.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-06 deposited with the CCDC.	2020-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.409(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.7995(4)
_cell_length_b                   12.8236(2)
_cell_length_c                   22.8740(4)
_cell_measurement_reflns_used    16669
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.6170
_cell_measurement_theta_min      4.0180
_cell_volume                     5953.2(2)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -82.00 -48.00   1.00    7.50    --  -37.08 -38.00  30.00   34
  2  ω     60.00 101.00   1.00    7.50    --   37.08  57.00-150.00   41
  3  ω     22.00  49.00   1.00    7.50    --   37.08 -57.00  60.00   27
  4  ω    -17.00  10.00   1.00    7.50    --   37.08 -57.00-150.00   27
  5  ω    -29.00  -3.00   1.00    7.50    --   37.08 -57.00  60.00   26
  6  ω     36.00  84.00   1.00    7.50    --   37.08-125.00-150.00   48
  7  ω     29.00  58.00   1.00    7.50    --   37.08  57.00-150.00   29
  8  ω     -8.00  65.00   1.00    7.50    --   37.08 -19.00 -90.00   73
  9  ω     15.00  51.00   1.00    7.50    --   37.08 -57.00-150.00   36
 10  ω     39.00  64.00   1.00    7.50    --   37.08 -77.00  60.00   25
 11  ω    -17.00  51.00   1.00    7.50    --   37.08 -38.00-120.00   68
 12  ω     34.00  61.00   1.00    7.50    --   37.08-125.00 150.00   27
 13  ω     86.00 136.00   1.00   30.00    --  111.00 -25.00 120.00   50
 14  ω    131.00 168.00   1.00   30.00    --  111.00  12.00  90.00   37
 15  ω    109.00 176.00   1.00   30.00    --  111.00  38.00 -30.00   67
 16  ω     68.00 118.00   1.00   30.00    --  111.00  12.00  90.00   50
 17  ω     63.00 109.00   1.00   30.00    --  111.00-111.00 150.00   46
 18  ω     43.00  86.00   1.00   30.00    --  111.00 -92.00-120.00   43
 19  ω     62.00 104.00   1.00   30.00    --  111.00 178.00 -30.00   42
 20  ω     42.00 104.00   1.00   30.00    --  111.00 -92.00-150.00   62
 21  ω     98.00 125.00   1.00   30.00    --  111.00 -38.00 -30.00   27
 22  ω    109.00 163.00   1.00   30.00    --  111.00 111.00 150.00   54
 23  ω     42.00  82.00   1.00   30.00    --  111.00 -38.00 -30.00   40
 24  ω    102.00 129.00   1.00   30.00    --  111.00  64.00 -60.00   27
 25  ω    150.00 176.00   1.00   30.00    --  111.00  64.00 -60.00   26
 26  ω     45.00  70.00   1.00   30.00    --  111.00-111.00   0.00   25
 27  ω     76.00 130.00   1.00   30.00    --  111.00 -66.00 -98.14   54
 28  ω     72.00 100.00   1.00   30.00    --  111.00 -77.00 120.00   28
 29  ω    100.00 133.00   1.00   30.00    --  111.00 -25.00 -30.00   33
 30  ω     80.00 105.00   1.00   30.00    --  111.00-111.00  30.00   25
 31  ω     48.00  75.00   1.00   30.00    --  111.00-111.00  30.00   27
 32  ω     81.00 106.00   1.00   30.00    --  111.00 -92.00-180.00   25
 33  ω     48.00  75.00   1.00   30.00    --  111.00 -92.00-180.00   27
 34  ω     71.00 119.00   1.00   30.00    --  111.00 -64.00 150.00   48
 35  ω    123.00 160.00   1.00   30.00    --  111.00  38.00-180.00   37
 36  ω     60.00 127.00   1.00   30.00    --  111.00 -50.00-180.00   67
 37  ω    104.00 177.00   1.00   30.00    --  111.00  77.00 -90.00   73
 38  ω    126.00 159.00   1.00   30.00    --  111.00  25.00 -60.00   33
 39  ω     50.00  89.00   1.00   30.00    --  111.00 -92.00 -90.00   39
 40  ω     56.00  81.00   1.00   30.00    --  111.00 -25.00 -30.00   25
 41  ω     81.00 106.00   1.00   30.00    --  111.00-111.00   0.00   25
 42  ω     84.00 109.00   1.00   30.00    --  111.00-111.00 120.00   25
 43  ω     56.00  83.00   1.00   30.00    --  111.00 -50.00-120.00   27
;
_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      0.0455167000
_diffrn_orient_matrix_UB_12      0.0063843000
_diffrn_orient_matrix_UB_13      -0.0379331000
_diffrn_orient_matrix_UB_21      0.0607153000
_diffrn_orient_matrix_UB_22      -0.0006429000
_diffrn_orient_matrix_UB_23      0.0615786000
_diffrn_orient_matrix_UB_31      0.0021370000
_diffrn_orient_matrix_UB_32      -0.1199338000
_diffrn_orient_matrix_UB_33      -0.0023991000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            45204
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.760
_diffrn_reflns_theta_min         4.024
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.556
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83182
_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 red'
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       plate
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.172
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.037
_refine_diff_density_max         2.886
_refine_diff_density_min         -1.940
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         11926
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0505
_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)+(0.0545P)²+29.4186P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1347
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9743
_reflns_number_total             11926
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0cc02070b3.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7126395--7126402.cif.'
_cod_original_cell_volume        5953.16(19)
_cod_database_code               7126402
_publcif_datablock.id            {22d23fa7-6121-4349-b642-2831eeb9a4c9}
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C52H52B1N6O2P2Br1W1Pd1
_chemical_oxdiff_usercomment     'Vap. Diff. n-hex into THF'
_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 98.01
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C11(H11), C16(H16), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25),
 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), C71(H71), C72(H72), C73(H73),
  C74(H74), C75(H75)
2.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)
;
_ins_header
;
TITL LB009_scale_filt in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  21.799505  12.823648  22.874023  90.0000 111.4086  90.0000
ZERR    4.00   0.000415   0.000209   0.000435   0.0000   0.0022   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H B N O P Br Pd W
UNIT 208.00 208.00 4.00 24.00 8.00 8.00 4.00 4.00 4.00
TREF
HKLF 4
END
;
_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 1.467
_oxdiff_exptl_absorpt_empirical_full_min 0.753
_publcif_funding_html
;
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.55413(2) 0.63560(2) 0.74728(2) 0.02516(8) Uani 1 1 d . . . . .
Pd1 Pd 0.43249(2) 0.58222(3) 0.66411(2) 0.02575(11) Uani 1 1 d . . . . .
Br1 Br 0.33897(3) 0.61473(6) 0.55965(3) 0.04176(18) Uani 1 1 d . . . . .
P1 P 0.48480(7) 0.81120(12) 0.62376(6) 0.0239(3) Uani 1 1 d . . . . .
P2 P 0.37166(7) 0.43580(13) 0.67545(7) 0.0286(3) Uani 1 1 d . . . . .
O1 O 0.5477(2) 0.4033(4) 0.7023(3) 0.0415(11) Uani 1 1 d . . . . .
O2 O 0.4561(3) 0.5732(5) 0.8139(2) 0.0496(14) Uani 1 1 d . . . . .
N1 N 0.6355(2) 0.5808(4) 0.8366(2) 0.0291(11) Uani 1 1 d . . . . .
N2 N 0.6905(2) 0.6411(4) 0.8630(2) 0.0286(11) Uani 1 1 d . . . . .
N3 N 0.5773(2) 0.7829(4) 0.8038(2) 0.0270(10) Uani 1 1 d . . . . .
N4 N 0.6410(3) 0.8180(5) 0.8325(2) 0.0329(12) Uani 1 1 d . . . . .
N5 N 0.6449(2) 0.6674(4) 0.7266(2) 0.0263(10) Uani 1 1 d . . . . .
N6 N 0.6956(2) 0.7275(4) 0.7663(2) 0.0281(11) Uani 1 1 d . . . . .
C1 C 0.4942(3) 0.7026(5) 0.6706(3) 0.0278(12) Uani 1 1 d . . . . .
C2 C 0.5454(3) 0.4892(5) 0.7153(3) 0.0305(13) Uani 1 1 d . . . . .
C3 C 0.4865(3) 0.5948(5) 0.7843(3) 0.0330(13) Uani 1 1 d . . . . .
C4 C 0.5941(4) 0.4099(6) 0.8613(4) 0.052(2) Uani 1 1 d . . . . .
H4A H 0.550568 0.439052 0.848338 0.078 Uiso 1 1 calc GR . . . .
H4B H 0.602671 0.369945 0.899005 0.078 Uiso 1 1 calc GR . . . .
H4C H 0.597236 0.365454 0.828795 0.078 Uiso 1 1 calc GR . . . .
C5 C 0.6434(3) 0.4957(5) 0.8736(3) 0.0359(14) Uani 1 1 d . . . . .
C6 C 0.7034(3) 0.5035(6) 0.9234(3) 0.0371(15) Uani 1 1 d . . . . .
H6 H 0.720889 0.455433 0.955659 0.045 Uiso 1 1 calc R . . . .
C7 C 0.7324(3) 0.5958(6) 0.9160(3) 0.0320(13) Uani 1 1 d . . . . .
C8 C 0.7960(3) 0.6415(6) 0.9560(3) 0.0412(16) Uani 1 1 d . . . . .
H8A H 0.822270 0.654952 0.931104 0.062 Uiso 1 1 calc GR . . . .
H8B H 0.818728 0.593553 0.989052 0.062 Uiso 1 1 calc GR . . . .
H8C H 0.788271 0.705600 0.973874 0.062 Uiso 1 1 calc GR . . . .
C9 C 0.4657(3) 0.8425(7) 0.7969(4) 0.0488(19) Uani 1 1 d . . . . .
H9A H 0.448983 0.814741 0.755013 0.073 Uiso 1 1 calc GR . . . .
H9B H 0.446668 0.909909 0.797177 0.073 Uiso 1 1 calc GR . . . .
H9C H 0.454245 0.796463 0.824447 0.073 Uiso 1 1 calc GR . . . .
C10 C 0.5392(3) 0.8522(6) 0.8188(3) 0.0349(14) Uani 1 1 d . . . . .
C11 C 0.5780(4) 0.9311(6) 0.8563(3) 0.0419(17) Uani 1 1 d . . . . .
H11 H 0.563338 0.988609 0.872342 0.050 Uiso 1 1 calc R . . . .
C12 C 0.6424(3) 0.9070(5) 0.8648(3) 0.0362(15) Uani 1 1 d . . . . .
C13 C 0.7044(4) 0.9640(7) 0.9006(4) 0.052(2) Uani 1 1 d . . . . .
H13A H 0.730425 0.923059 0.936176 0.078 Uiso 1 1 calc GR . . . .
H13B H 0.693859 1.029635 0.914822 0.078 Uiso 1 1 calc GR . . . .
H13C H 0.728969 0.976001 0.873908 0.078 Uiso 1 1 calc GR . . . .
C14 C 0.6228(3) 0.5717(5) 0.6260(3) 0.0351(14) Uani 1 1 d . . . . .
H14A H 0.626070 0.500807 0.640240 0.053 Uiso 1 1 calc GR . . . .
H14B H 0.638196 0.576552 0.591750 0.053 Uiso 1 1 calc GR . . . .
H14C H 0.577610 0.593841 0.612067 0.053 Uiso 1 1 calc GR . . . .
C15 C 0.6638(3) 0.6401(5) 0.6785(3) 0.0291(12) Uani 1 1 d . . . . .
C16 C 0.7239(3) 0.6849(5) 0.6862(3) 0.0321(13) Uani 1 1 d . . . . .
H16 H 0.747045 0.678868 0.659353 0.038 Uiso 1 1 calc R . . . .
C17 C 0.7429(3) 0.7405(5) 0.7420(3) 0.0321(13) Uani 1 1 d . . . . .
C18 C 0.8028(3) 0.8027(7) 0.7730(4) 0.0455(18) Uani 1 1 d . . . . .
H18A H 0.790746 0.873611 0.777103 0.068 Uiso 1 1 calc GR . . . .
H18B H 0.830123 0.800764 0.748274 0.068 Uiso 1 1 calc GR . . . .
H18C H 0.826607 0.774409 0.813902 0.068 Uiso 1 1 calc GR . . . .
C20 C 0.4712(3) 0.7826(5) 0.5424(3) 0.0255(11) Uani 1 1 d . . . . .
C21 C 0.4642(3) 0.8647(6) 0.5008(3) 0.0347(14) Uani 1 1 d . . . . .
H21 H 0.465314 0.933011 0.514872 0.042 Uiso 1 1 calc R . . . .
C22 C 0.4555(3) 0.8459(7) 0.4385(3) 0.0414(17) Uani 1 1 d . . . . .
H22 H 0.450380 0.901106 0.410711 0.050 Uiso 1 1 calc R . . . .
C23 C 0.4546(3) 0.7438(7) 0.4181(3) 0.048(2) Uani 1 1 d . . . . .
H23 H 0.449850 0.730375 0.376701 0.058 Uiso 1 1 calc R . . . .
C24 C 0.4608(3) 0.6625(6) 0.4590(3) 0.0435(17) Uani 1 1 d . . . . .
H24 H 0.459664 0.594175 0.444967 0.052 Uiso 1 1 calc R . . . .
C25 C 0.4688(3) 0.6817(6) 0.5215(3) 0.0349(14) Uani 1 1 d . . . . .
H25 H 0.472526 0.626334 0.548861 0.042 Uiso 1 1 calc R . . . .
C30 C 0.5586(3) 0.8909(5) 0.6497(3) 0.0269(12) Uani 1 1 d . . . . .
C31 C 0.6055(3) 0.8803(5) 0.6217(3) 0.0324(13) Uani 1 1 d . . . . .
H31 H 0.597847 0.834525 0.588184 0.039 Uiso 1 1 calc R . . . .
C32 C 0.6637(3) 0.9379(5) 0.6436(3) 0.0369(15) Uani 1 1 d . . . . .
H32 H 0.695215 0.929583 0.625432 0.044 Uiso 1 1 calc R . . . .
C33 C 0.6746(3) 1.0078(5) 0.6927(3) 0.0367(15) Uani 1 1 d . . . . .
H33 H 0.712829 1.047720 0.706776 0.044 Uiso 1 1 calc R . . . .
C34 C 0.6286(3) 1.0178(6) 0.7206(3) 0.0379(15) Uani 1 1 d . . . . .
H34 H 0.636743 1.063303 0.754265 0.045 Uiso 1 1 calc R . . . .
C35 C 0.5704(3) 0.9611(5) 0.6994(3) 0.0332(13) Uani 1 1 d . . . . .
H35 H 0.539412 0.969787 0.718181 0.040 Uiso 1 1 calc R . . . .
C40 C 0.4176(3) 0.8959(5) 0.6245(3) 0.0303(13) Uani 1 1 d . . . . .
C41 C 0.4159(3) 1.0002(6) 0.6095(3) 0.0380(15) Uani 1 1 d . . . . .
H41 H 0.450796 1.029892 0.601134 0.046 Uiso 1 1 calc R . . . .
C42 C 0.3623(4) 1.0611(6) 0.6069(4) 0.0469(18) Uani 1 1 d . . . . .
H42 H 0.361905 1.131815 0.597824 0.056 Uiso 1 1 calc R . . . .
C43 C 0.3098(4) 1.0173(7) 0.6175(4) 0.051(2) Uani 1 1 d . . . . .
H43 H 0.273703 1.058254 0.615016 0.061 Uiso 1 1 calc R . . . .
C44 C 0.3105(4) 0.9143(7) 0.6317(4) 0.0467(18) Uani 1 1 d . . . . .
H44 H 0.274678 0.885378 0.638705 0.056 Uiso 1 1 calc R . . . .
C45 C 0.3648(3) 0.8505(6) 0.6359(3) 0.0357(14) Uani 1 1 d . . . . .
H45 H 0.365395 0.780131 0.645983 0.043 Uiso 1 1 calc R . . . .
C50 C 0.3411(3) 0.3616(5) 0.6020(3) 0.0330(13) Uani 1 1 d . . . . .
C51 C 0.2764(4) 0.3259(6) 0.5733(3) 0.0413(16) Uani 1 1 d . . . . .
H51 H 0.246057 0.335831 0.592669 0.050 Uiso 1 1 calc R . . . .
C52 C 0.2575(4) 0.2752(7) 0.5153(4) 0.052(2) Uani 1 1 d . . . . .
H52 H 0.214202 0.252608 0.495813 0.063 Uiso 1 1 calc R . . . .
C53 C 0.3026(5) 0.2585(7) 0.4868(3) 0.053(2) Uani 1 1 d . . . . .
H53 H 0.289595 0.224893 0.448133 0.064 Uiso 1 1 calc R . . . .
C54 C 0.3668(5) 0.2914(7) 0.5155(4) 0.053(2) Uani 1 1 d . . . . .
H54 H 0.397545 0.277757 0.497073 0.064 Uiso 1 1 calc R . . . .
C55 C 0.3854(4) 0.3448(6) 0.5718(3) 0.0421(16) Uani 1 1 d . . . . .
H55 H 0.428202 0.369933 0.589938 0.051 Uiso 1 1 calc R . . . .
C60 C 0.2986(3) 0.4724(6) 0.6923(3) 0.0372(15) Uani 1 1 d . . . . .
C61 C 0.2813(4) 0.5753(7) 0.6913(4) 0.053(2) Uani 1 1 d . . . . .
H61 H 0.306342 0.625862 0.681160 0.064 Uiso 1 1 calc R . . . .
C62 C 0.2268(5) 0.6052(9) 0.7053(6) 0.077(3) Uani 1 1 d . . . . .
H62 H 0.216137 0.675425 0.705181 0.093 Uiso 1 1 calc R . . . .
C63 C 0.1892(5) 0.5316(10) 0.7192(5) 0.075(3) Uani 1 1 d . . . . .
H63 H 0.152517 0.551806 0.727973 0.090 Uiso 1 1 calc R . . . .
C64 C 0.2052(4) 0.4271(10) 0.7204(5) 0.066(3) Uani 1 1 d . . . . .
H64 H 0.179563 0.377120 0.730136 0.080 Uiso 1 1 calc R . . . .
C65 C 0.2600(4) 0.3970(7) 0.7068(4) 0.0470(18) Uani 1 1 d . . . . .
H65 H 0.270855 0.326788 0.707450 0.056 Uiso 1 1 calc R . . . .
C70 C 0.4091(3) 0.3352(5) 0.7351(3) 0.0330(13) Uani 1 1 d . . . . .
C71 C 0.4075(4) 0.3437(7) 0.7950(4) 0.0457(17) Uani 1 1 d . . . . .
H71 H 0.384288 0.398351 0.804083 0.055 Uiso 1 1 calc R . . . .
C72 C 0.4397(4) 0.2724(7) 0.8416(4) 0.052(2) Uani 1 1 d . . . . .
H72 H 0.438146 0.279929 0.881507 0.063 Uiso 1 1 calc R . . . .
C73 C 0.4743(5) 0.1896(6) 0.8292(4) 0.053(2) Uani 1 1 d . . . . .
H73 H 0.495488 0.140758 0.860049 0.063 Uiso 1 1 calc R . . . .
C74 C 0.4763(5) 0.1823(6) 0.7700(4) 0.054(2) Uani 1 1 d . . . . .
H74 H 0.500296 0.128336 0.761482 0.064 Uiso 1 1 calc R . . . .
C75 C 0.4442(4) 0.2515(5) 0.7230(4) 0.0403(15) Uani 1 1 d . . . . .
H75 H 0.445708 0.242824 0.683180 0.048 Uiso 1 1 calc R . . . .
B1 B 0.6983(3) 0.7477(6) 0.8335(3) 0.0304(14) Uani 1 1 d . . . . .
H1 H 0.740372 0.780056 0.858684 0.036 Uiso 1 1 calc R . . . .
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'
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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 '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
-2 -8 -3 0.0541
7 4 8 0.0535
-6 6 -6 0.0638
7 -3 8 0.0530
12 0 -12 0.0239
-12 -1 12 0.0110
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
N1 W1 Pd1 142.22(14) . . ?
N3 W1 Pd1 124.84(12) . . ?
N3 W1 N1 78.71(19) . . ?
N5 W1 Pd1 127.54(12) . . ?
N5 W1 N1 77.61(18) . . ?
N5 W1 N3 86.45(19) . . ?
C1 W1 Pd1 47.56(18) . . ?
C1 W1 N1 170.2(2) . . ?
C1 W1 N3 94.8(2) . . ?
C1 W1 N5 94.8(2) . . ?
C1 W1 C2 98.1(2) . . ?
C1 W1 C3 97.9(3) . . ?
C2 W1 Pd1 64.58(17) . . ?
C2 W1 N1 88.7(2) . . ?
C2 W1 N3 167.1(2) . . ?
C2 W1 N5 93.8(2) . . ?
C2 W1 C3 85.7(3) . . ?
C3 W1 Pd1 63.56(18) . . ?
C3 W1 N1 89.6(2) . . ?
C3 W1 N3 91.2(2) . . ?
C3 W1 N5 167.2(2) . . ?
Br1 Pd1 W1 148.78(3) . . ?
Br1 Pd1 C2 143.17(15) . . ?
Br1 Pd1 C3 152.96(16) . . ?
P2 Pd1 W1 124.31(4) . . ?
P2 Pd1 Br1 86.79(4) . . ?
P2 Pd1 C2 93.63(14) . . ?
P2 Pd1 C3 89.37(15) . . ?
C1 Pd1 W1 45.89(17) . . ?
C1 Pd1 Br1 103.17(17) . . ?
C1 Pd1 P2 169.82(17) . . ?
C1 Pd1 C2 79.7(2) . . ?
C1 Pd1 C3 80.8(2) . . ?
C2 Pd1 W1 44.00(13) . . ?
C3 Pd1 W1 44.66(14) . . ?
C3 Pd1 C2 63.8(2) . . ?
C1 P1 C20 114.4(3) . . ?
C1 P1 C30 111.3(3) . . ?
C1 P1 C40 112.8(3) . . ?
C20 P1 C30 104.1(3) . . ?
C20 P1 C40 107.4(3) . . ?
C30 P1 C40 106.3(3) . . ?
C50 P2 Pd1 110.0(2) . . ?
C50 P2 C70 103.4(3) . . ?
C60 P2 Pd1 112.6(3) . . ?
C60 P2 C50 105.8(3) . . ?
C60 P2 C70 102.1(3) . . ?
C70 P2 Pd1 121.5(2) . . ?
N2 N1 W1 119.5(4) . . ?
C5 N1 W1 133.7(4) . . ?
C5 N1 N2 106.8(5) . . ?
N1 N2 B1 121.4(5) . . ?
C7 N2 N1 110.4(5) . . ?
C7 N2 B1 128.2(5) . . ?
N4 N3 W1 121.8(4) . . ?
C10 N3 W1 132.5(4) . . ?
C10 N3 N4 105.8(5) . . ?
N3 N4 B1 119.2(5) . . ?
C12 N4 N3 110.8(5) . . ?
C12 N4 B1 129.1(5) . . ?
N6 N5 W1 121.5(4) . . ?
C15 N5 W1 132.9(4) . . ?
C15 N5 N6 105.7(5) . . ?
N5 N6 B1 118.6(5) . . ?
C17 N6 N5 110.4(5) . . ?
C17 N6 B1 129.5(5) . . ?
W1 C1 Pd1 86.5(3) . . ?
P1 C1 W1 143.0(3) . . ?
P1 C1 Pd1 130.4(3) . . ?
W1 C2 Pd1 71.42(19) . . ?
O1 C2 W1 171.9(5) . . ?
O1 C2 Pd1 116.6(4) . . ?
W1 C3 Pd1 71.8(2) . . ?
O2 C3 W1 169.4(5) . . ?
O2 C3 Pd1 118.7(5) . . ?
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 124.0(6) . . ?
N1 C5 C6 108.7(6) . . ?
C6 C5 C4 127.3(6) . . ?
C5 C6 H6 126.3 . . ?
C7 C6 C5 107.3(6) . . ?
C7 C6 H6 126.3 . . ?
N2 C7 C6 106.8(6) . . ?
N2 C7 C8 124.0(6) . . ?
C6 C7 C8 129.2(6) . . ?
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 123.0(6) . . ?
N3 C10 C11 110.1(6) . . ?
C11 C10 C9 126.9(7) . . ?
C10 C11 H11 126.8 . . ?
C12 C11 C10 106.3(6) . . ?
C12 C11 H11 126.8 . . ?
N4 C12 C11 107.0(6) . . ?
N4 C12 C13 123.2(7) . . ?
C11 C12 C13 129.8(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 122.4(6) . . ?
N5 C15 C16 110.2(6) . . ?
C16 C15 C14 127.4(6) . . ?
C15 C16 H16 126.8 . . ?
C15 C16 C17 106.3(6) . . ?
C17 C16 H16 126.8 . . ?
N6 C17 C16 107.4(6) . . ?
N6 C17 C18 123.0(6) . . ?
C16 C17 C18 129.5(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 . . ?
C21 C20 P1 119.1(5) . . ?
C25 C20 P1 121.3(5) . . ?
C25 C20 C21 119.6(6) . . ?
C20 C21 H21 119.6 . . ?
C20 C21 C22 120.7(7) . . ?
C22 C21 H21 119.6 . . ?
C21 C22 H22 120.4 . . ?
C23 C22 C21 119.2(7) . . ?
C23 C22 H22 120.4 . . ?
C22 C23 H23 119.9 . . ?
C24 C23 C22 120.1(6) . . ?
C24 C23 H23 119.9 . . ?
C23 C24 H24 119.8 . . ?
C23 C24 C25 120.5(7) . . ?
C25 C24 H24 119.8 . . ?
C20 C25 C24 119.8(7) . . ?
C20 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
C31 C30 P1 120.4(5) . . ?
C31 C30 C35 119.1(6) . . ?
C35 C30 P1 120.5(5) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 C30 120.3(6) . . ?
C32 C31 H31 119.8 . . ?
C31 C32 H32 120.1 . . ?
C33 C32 C31 119.9(7) . . ?
C33 C32 H32 120.1 . . ?
C32 C33 H33 120.1 . . ?
C34 C33 C32 119.8(6) . . ?
C34 C33 H33 120.1 . . ?
C33 C34 H34 119.4 . . ?
C33 C34 C35 121.1(6) . . ?
C35 C34 H34 119.4 . . ?
C30 C35 H35 120.2 . . ?
C34 C35 C30 119.7(6) . . ?
C34 C35 H35 120.2 . . ?
C41 C40 P1 121.4(5) . . ?
C41 C40 C45 120.2(6) . . ?
C45 C40 P1 118.2(5) . . ?
C40 C41 H41 120.0 . . ?
C40 C41 C42 120.1(7) . . ?
C42 C41 H41 120.0 . . ?
C41 C42 H42 119.8 . . ?
C43 C42 C41 120.4(7) . . ?
C43 C42 H42 119.8 . . ?
C42 C43 H43 120.0 . . ?
C44 C43 C42 120.1(7) . . ?
C44 C43 H43 120.0 . . ?
C43 C44 H44 119.5 . . ?
C43 C44 C45 121.0(8) . . ?
C45 C44 H44 119.5 . . ?
C40 C45 C44 118.2(7) . . ?
C40 C45 H45 120.9 . . ?
C44 C45 H45 120.9 . . ?
C51 C50 P2 124.6(6) . . ?
C55 C50 P2 116.6(5) . . ?
C55 C50 C51 118.7(6) . . ?
C50 C51 H51 120.1 . . ?
C52 C51 C50 119.8(7) . . ?
C52 C51 H51 120.1 . . ?
C51 C52 H52 119.8 . . ?
C53 C52 C51 120.4(7) . . ?
C53 C52 H52 119.8 . . ?
C52 C53 H53 119.9 . . ?
C54 C53 C52 120.1(7) . . ?
C54 C53 H53 119.9 . . ?
C53 C54 H54 120.1 . . ?
C53 C54 C55 119.8(8) . . ?
C55 C54 H54 120.1 . . ?
C50 C55 H55 119.4 . . ?
C54 C55 C50 121.2(7) . . ?
C54 C55 H55 119.4 . . ?
C61 C60 P2 119.9(6) . . ?
C61 C60 C65 118.9(7) . . ?
C65 C60 P2 121.2(6) . . ?
C60 C61 H61 119.5 . . ?
C60 C61 C62 120.9(9) . . ?
C62 C61 H61 119.5 . . ?
C61 C62 H62 120.0 . . ?
C63 C62 C61 120.0(10) . . ?
C63 C62 H62 120.0 . . ?
C62 C63 H63 119.8 . . ?
C62 C63 C64 120.5(8) . . ?
C64 C63 H63 119.8 . . ?
C63 C64 H64 120.2 . . ?
C63 C64 C65 119.7(9) . . ?
C65 C64 H64 120.2 . . ?
C60 C65 H65 120.0 . . ?
C64 C65 C60 120.0(9) . . ?
C64 C65 H65 120.0 . . ?
C71 C70 P2 120.9(6) . . ?
C71 C70 C75 117.8(7) . . ?
C75 C70 P2 121.2(5) . . ?
C70 C71 H71 119.4 . . ?
C72 C71 C70 121.3(8) . . ?
C72 C71 H71 119.4 . . ?
C71 C72 H72 119.7 . . ?
C71 C72 C73 120.5(8) . . ?
C73 C72 H72 119.7 . . ?
C72 C73 H73 121.0 . . ?
C74 C73 C72 117.9(8) . . ?
C74 C73 H73 121.0 . . ?
C73 C74 H74 118.7 . . ?
C75 C74 C73 122.5(8) . . ?
C75 C74 H74 118.7 . . ?
C70 C75 H75 120.0 . . ?
C74 C75 C70 119.9(7) . . ?
C74 C75 H75 120.0 . . ?
N2 B1 H1 110.1 . . ?
N4 B1 N2 107.8(6) . . ?
N4 B1 N6 110.6(5) . . ?
N4 B1 H1 110.1 . . ?
N6 B1 N2 108.2(5) . . ?
N6 B1 H1 110.1 . . ?
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
W1 Pd1 2.7271(5) . ?
W1 N1 2.273(4) . ?
W1 N3 2.240(5) . ?
W1 N5 2.233(5) . ?
W1 C1 1.962(6) . ?
W1 C2 1.998(6) . ?
W1 C3 2.018(7) . ?
Pd1 Br1 2.5461(7) . ?
Pd1 P2 2.3670(16) . ?
Pd1 C1 2.016(6) . ?
Pd1 C2 2.598(6) . ?
Pd1 C3 2.571(6) . ?
P1 C1 1.724(6) . ?
P1 C20 1.811(6) . ?
P1 C30 1.813(6) . ?
P1 C40 1.829(7) . ?
P2 C50 1.832(6) . ?
P2 C60 1.832(7) . ?
P2 C70 1.838(7) . ?
O1 C2 1.147(8) . ?
O2 C3 1.142(8) . ?
N1 N2 1.368(7) . ?
N1 C5 1.353(8) . ?
N2 C7 1.353(8) . ?
N2 B1 1.560(9) . ?
N3 N4 1.377(7) . ?
N3 C10 1.344(8) . ?
N4 C12 1.354(9) . ?
N4 B1 1.534(9) . ?
N5 N6 1.380(7) . ?
N5 C15 1.354(8) . ?
N6 C17 1.347(9) . ?
N6 B1 1.540(9) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C4 C5 1.491(9) . ?
C5 C6 1.390(9) . ?
C6 H6 0.9300 . ?
C6 C7 1.381(10) . ?
C7 C8 1.475(9) . ?
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 1.499(9) . ?
C10 C11 1.395(10) . ?
C11 H11 0.9300 . ?
C11 C12 1.380(10) . ?
C12 C13 1.492(9) . ?
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 1.494(9) . ?
C15 C16 1.382(9) . ?
C16 H16 0.9300 . ?
C16 C17 1.386(9) . ?
C17 C18 1.474(9) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C20 C21 1.390(9) . ?
C20 C25 1.374(9) . ?
C21 H21 0.9300 . ?
C21 C22 1.390(9) . ?
C22 H22 0.9300 . ?
C22 C23 1.387(12) . ?
C23 H23 0.9300 . ?
C23 C24 1.374(12) . ?
C24 H24 0.9300 . ?
C24 C25 1.398(10) . ?
C25 H25 0.9300 . ?
C30 C31 1.398(9) . ?
C30 C35 1.399(9) . ?
C31 H31 0.9300 . ?
C31 C32 1.395(9) . ?
C32 H32 0.9300 . ?
C32 C33 1.388(10) . ?
C33 H33 0.9300 . ?
C33 C34 1.376(11) . ?
C34 H34 0.9300 . ?
C34 C35 1.387(9) . ?
C35 H35 0.9300 . ?
C40 C41 1.379(10) . ?
C40 C45 1.395(10) . ?
C41 H41 0.9300 . ?
C41 C42 1.389(10) . ?
C42 H42 0.9300 . ?
C42 C43 1.374(12) . ?
C43 H43 0.9300 . ?
C43 C44 1.358(12) . ?
C44 H44 0.9300 . ?
C44 C45 1.414(9) . ?
C45 H45 0.9300 . ?
C50 C51 1.398(9) . ?
C50 C55 1.393(10) . ?
C51 H51 0.9300 . ?
C51 C52 1.396(10) . ?
C52 H52 0.9300 . ?
C52 C53 1.381(13) . ?
C53 H53 0.9300 . ?
C53 C54 1.377(12) . ?
C54 H54 0.9300 . ?
C54 C55 1.383(10) . ?
C55 H55 0.9300 . ?
C60 C61 1.370(12) . ?
C60 C65 1.400(10) . ?
C61 H61 0.9300 . ?
C61 C62 1.392(12) . ?
C62 H62 0.9300 . ?
C62 C63 1.361(16) . ?
C63 H63 0.9300 . ?
C63 C64 1.383(16) . ?
C64 H64 0.9300 . ?
C64 C65 1.392(11) . ?
C65 H65 0.9300 . ?
C70 C71 1.390(10) . ?
C70 C75 1.403(10) . ?
C71 H71 0.9300 . ?
C71 C72 1.385(11) . ?
C72 H72 0.9300 . ?
C72 C73 1.391(12) . ?
C73 H73 0.9300 . ?
C73 C74 1.374(12) . ?
C74 H74 0.9300 . ?
C74 C75 1.373(11) . ?
C75 H75 0.9300 . ?
B1 H1 0.9800 . ?
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
-1.7483 -7.9283 -3.1849 -0.0094 -0.2972 0.9548
6.6227 3.7554 7.9626 0.0234 0.8900 -0.4553
-5.8192 5.9693 -5.5497 -0.0162 -0.6989 -0.7150
7.4720 -2.8489 7.8777 0.0231 0.9406 0.3387
11.8408 0.3776 -12.0811 0.9996 -0.0253 0.0090
-11.8298 -0.5292 12.0687 -0.9996 0.0253 0.0092
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.866 0.500 713.4 120.1 ?
2 0.500 -0.020 0.000 713.4 120.1 ?
