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_7704528
_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         'C51 H59 B2 N12 O2 P Pt W'
_chemical_formula_sum            'C51 H59 B2 N12 O2 P Pt W'
_chemical_formula_weight         1303.63
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                71.254(2)
_cell_angle_beta                 79.943(2)
_cell_angle_gamma                82.947(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8902(2)
_cell_length_b                   15.0338(4)
_cell_length_c                   17.0497(4)
_cell_measurement_reflns_used    13801
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.6000
_cell_measurement_theta_min      5.2790
_cell_volume                     2596.04(11)
_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 (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 0.996
_diffrn_measured_fraction_theta_max 0.977
_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    -63.00  31.00   1.00    1.00    --  -36.95  19.00-120.00   94
  2  \w     29.00  87.00   1.00    1.00    --   36.95-125.00-150.00   58
  3  \w      2.00  54.00   1.00    1.00    --   36.95 -38.00-150.00   52
  4  \w     16.00  76.00   1.00    1.00    --   36.95 -99.00  60.00   60
  5  \w    -33.00  65.00   1.00    1.00    --   36.95 -19.00  30.00   98
  6  \w    -30.00  53.00   1.00    1.00    --   36.95 -57.00 -30.00   83
  7  \w     49.00 106.00   1.00    1.00    --   36.95-160.00  27.00   57
  8  \w    -32.00  -3.00   1.00    1.00    --   36.95 -38.00-150.00   29
  9  \w     43.00  95.00   1.00    1.00    --  111.00 -25.00 -60.00   52
 10  \w     51.00 101.00   1.00    1.00    --  111.00 -92.00   0.00   50
 11  \w     48.00 126.00   1.00    1.00    --  111.00 -50.00 -30.00   78
 12  \w     52.00 117.00   1.00    1.00    --  111.00 -64.00-120.00   65
 13  \w     92.00 175.00   1.00    1.00    --  111.00  25.00-150.00   83
 14  \w    106.00 178.00   1.00    1.00    --  111.00  50.00-120.00   72
 15  \w     49.00 129.00   1.00    1.00    --  111.00 -64.00 150.00   80
 16  \w    117.00 170.00   1.00    1.00    --  111.00  77.00 -60.00   53
 17  \w     41.00 101.00   1.00    1.00    --  111.00-111.00 150.00   60
 18  \w     45.00 105.00   1.00    1.00    --  111.00 -38.00 150.00   60
 19  \w     69.00 109.00   1.00    1.00    --  111.00-111.00  90.00   40
 20  \w     60.00 109.00   1.00    1.00    --  111.00-111.00-180.00   49
 21  \w    102.00 136.00   1.00    1.00    --  111.00 -25.00 -60.00   34
 22  \w     41.00 133.00   1.00    1.00    --  111.00 -25.00-150.00   92
 23  \w    111.00 174.00   1.00    1.00    --  111.00  77.00 -90.00   63
 24  \w     79.00 108.00   1.00    1.00    --  111.00-111.00 -90.00   29
 25  \w     80.00 109.00   1.00    1.00    --  111.00-111.00   0.00   29
 26  \w     50.00  75.00   1.00    1.00    --  111.00-111.00   0.00   25
;
_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      -0.0122772000
_diffrn_orient_matrix_UB_12      0.0459527000
_diffrn_orient_matrix_UB_13      0.0700479000
_diffrn_orient_matrix_UB_21      -0.0459764000
_diffrn_orient_matrix_UB_22      -0.0917928000
_diffrn_orient_matrix_UB_23      0.0648569000
_diffrn_orient_matrix_UB_31      0.1359509000
_diffrn_orient_matrix_UB_32      -0.0351114000
_diffrn_orient_matrix_UB_33      0.0135656000
_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  0.0243
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19474
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.768
_diffrn_reflns_theta_min         3.472
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.705
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60171
_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 yellow'
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_description       block
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.061
_refine_diff_density_max         1.288
_refine_diff_density_min         -1.152
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         10286
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0222
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+1.2120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0572
_refine_ls_wR_factor_ref         0.0581
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9765
_reflns_number_total             10286
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01617a2.cif
_cod_data_source_block           12
_cod_depositor_comments
'Adding full bibliography for 7704524--7704531.cif.'
_cod_database_code               7704528
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C51 H60 B2 N12 O2 P1 Pt1 W1'
_chemical_oxdiff_usercomment     'Vap. Diff. Et2O/CH2Cl2 @ 0 degC'
_reflns_odcompleteness_completeness 99.11
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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. Restrained distances
 B2-H2 = B1-H1
 1.15 with sigma of 0.02
3. Rigid bond restraints
 W1, C1, Pt1
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
W1 \\sim C1 \\sim Pt1: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 2A
5.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C11(H11), C16(H16), C22(H22), C27(H27), C32(H32), 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)
5.b 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), C20(H20A,H20B,H20C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C34(H34A,
 H34B,H34C)
;
_shelx_res_checksum              34827
_ins_header
;
TITL LB011_scale in P1 
REM P1 (#1 in standard setting)
CELL 1.54184  10.890240  15.033785  17.049651  71.2540  79.9427  82.9470
ZERR    2.00   0.000168   0.000371   0.000445   0.0023   0.0017   0.0016
LATT -1
SFAC C H B N O P W Pt
UNIT 102.00 120.00 4.00 24.00 4.00 2.00 2.00 2.00
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 1.573
_oxdiff_exptl_absorpt_empirical_full_min 0.782