Heterobimetallic μ<sub>2</sub>-carbido complexes of platinum and tungsten.
Burt, Liam K.; Hill, Anthony F.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 8143–8161; doi:10.1039/d0dt01617a

data_7704524
_publ_section_title
;
 Heterobimetallic \m<sub>2</sub>-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  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -104.00 -20.00   1.00    1.15    --  -36.95 -57.00-180.00   84
  2  \w      5.00  31.00   1.00    1.15    --   36.95  86.00 -81.97   26
  3  \w      6.00  76.00   1.00    1.15    --   36.95 -99.00   0.00   70
  4  \w      3.00  29.00   1.00    1.15    --   36.95  90.00-171.38   26
  5  \w    -32.00 106.00   1.00    1.15    --   36.95   0.00   0.00  138
  6  \w     10.00  42.00   1.00    1.15    --   36.95  78.00 -54.12   32
  7  \w     18.00 106.00   1.00    1.15    --   36.95  38.00 150.00   88
  8  \w     20.00 104.00   1.00    1.15    --   36.95  57.00-180.00   84
  9  \w     20.00 104.00   1.00    1.15    --   36.95  57.00 -30.00   84
 10  \w    -21.00  64.00   1.00    1.15    --   36.95 -77.00   0.00   85
 11  \w     27.00  90.00   1.00    1.15    --   36.95-125.00  90.00   63
 12  \w     41.00 136.00   1.00    4.61    --  111.00 -25.00  90.00   95
 13  \w     42.00 106.00   1.00    4.61    --  111.00 -92.00   0.00   64
 14  \w     86.00 178.00   1.00    4.61    --  111.00  25.00 -30.00   92
 15  \w     41.00 109.00   1.00    4.61    --  111.00-111.00-180.00   68
 16  \w     41.00 109.00   1.00    4.61    --  111.00-111.00  60.00   68
 17  \w     41.00 109.00   1.00    4.61    --  111.00-111.00  90.00   68
 18  \w     41.00 109.00   1.00    4.61    --  111.00-111.00-150.00   68
 19  \w     61.00 146.00   1.00    4.61    --  111.00 178.00-180.00   85
 20  \w     61.00 146.00   1.00    4.61    --  111.00 178.00 -30.00   85
 21  \w     42.00 106.00   1.00    4.61    --  111.00 -92.00-180.00   64
 22  \w     44.00 131.00   1.00    4.61    --  111.00 -64.00-120.00   87
 23  \w     61.00 146.00   1.00    4.61    --  111.00 178.00   0.00   85
 24  \w     91.00 178.00   1.00    4.61    --  111.00  64.00 -90.00   87
 25  \w     92.00 178.00   1.00    4.61    --  111.00  38.00   0.00   86
 26  \w     41.00 109.00   1.00    4.61    --  111.00-111.00 -30.00   68
 27  \w     43.00 138.00   1.00    4.61    --  111.00 -77.00  90.00   95
 28  \w     65.00 178.00   1.00    4.61    --  111.00  12.00 -60.00  113
 29  \w     42.00 130.00   1.00    4.61    --  111.00 -38.00 150.00   88
 30  \w     44.00 131.00   1.00    4.61    --  111.00 -64.00  90.00   87
 31  \w     41.00 157.00   1.00    4.61    --  111.00 -12.00  90.00  116
 32  \w     43.00 138.00   1.00    4.61    --  111.00 -77.00-150.00   95
 33  \w     42.00 130.00   1.00    4.61    --  111.00 -38.00  90.00   88
 34  \w     41.00 109.00   1.00    4.61    --  111.00-111.00 -90.00   68
 35  \w     43.00 138.00   1.00    4.61    --  111.00 -77.00  30.00   95
 36  \w     41.00 157.00   1.00    4.61    --  111.00 -12.00 -30.00  116
 37  \w     41.00 109.00   1.00    4.61    --  111.00-111.00  30.00   68
 38  \w     42.00 106.00   1.00    4.61    --  111.00 -92.00  90.00   64
 39  \w     41.00 109.00   1.00    4.61    --  111.00-111.00 150.00   68
 40  \w     41.00 109.00   1.00    4.61    --  111.00-111.00 120.00   68
 41  \w     42.00 106.00   1.00    4.61    --  111.00 -92.00 -30.00   64
 42  \w     43.00 128.00   1.00    4.61    --  111.00 -50.00 -60.00   85
 43  \w     92.00 178.00   1.00    4.61    --  111.00  38.00 120.00   86
 44  \w     43.00 138.00   1.00    4.61    --  111.00 -77.00 -60.00   95
 45  \w     42.00 130.00   1.00    4.61    --  111.00 -38.00 -60.00   88
 46  \w     42.00 130.00   1.00    4.61    --  111.00 -38.00-150.00   88
 47  \w     41.00 109.00   1.00    4.61    --  111.00-111.00-120.00   68
 48  \w    103.00 178.00   1.00    4.61    --  111.00  77.00-120.00   75
 49  \w     42.00 106.00   1.00    4.61    --  111.00 -92.00  30.00   64
 50  \w     44.00 131.00   1.00    4.61    --  111.00 -64.00 -90.00   87
 51  \w     40.00 139.00   1.00    4.61    --  111.00 -21.00 -51.35   99
 52  \w    -21.00  64.00   1.00    1.15    --   36.95 -77.00-120.00   85
 53  \w      4.00  30.00   1.00    1.15    --   36.95  89.00  64.31   26
 54  \w    -30.00  54.00   1.00    1.15    --   36.95 -57.00-180.00   84
 55  \w      4.00  30.00   1.00    1.15    --   36.95  88.00  -5.20   26
 56  \w      5.00  31.00   1.00    1.15    --   36.95  87.00 106.37   26
 57  \w    -32.00  56.00   1.00    1.15    --   36.95 -38.00-120.00   88
 58  \w    -32.00  56.00   1.00    1.15    --   36.95 -38.00  90.00   88
 59  \w     20.00 104.00   1.00    1.15    --   36.95  57.00  90.00   84
 60  \w     20.00 104.00   1.00    1.15    --   36.95  57.00 150.00   84
 61  \w     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       '\w 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/[\s^2^(Fo^2^)+(0.0558P)^2^+1.7696P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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'
_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)
;
_shelx_res_checksum              4671
_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