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_7704527
_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         'C54 H61 B N8 O2 P Pt W, F6 P'
_chemical_formula_sum            'C54 H61 B F6 N8 O2 P2 Pt W'
_chemical_formula_weight         1419.79
_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                79.857(3)
_cell_angle_beta                 86.505(2)
_cell_angle_gamma                75.021(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6701(3)
_cell_length_b                   11.7291(4)
_cell_length_c                   21.3711(7)
_cell_measurement_reflns_used    15040
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.3610
_cell_measurement_theta_min      3.7110
_cell_volume                     2781.34(15)
_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 5.1872
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.810
_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    -15.00  28.00   1.00   25.00    --  -10.52 -99.00 -30.00   43
  2  \w    -30.00  -4.00   1.00   25.00    --  -10.52  77.00 -60.00   26
  3  \w    -11.00  15.00   1.00   25.00    --  -10.52 -99.00 120.00   26
  4  \w     17.00  51.00   1.00   25.00    --   10.91 -99.00 -90.00   34
  5  \w    -47.00  33.00   1.00   25.00    --   10.91 -57.00  90.00   80
  6  \w    -61.00  85.00   1.00   25.00    --   10.91   0.00 120.00  146
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0191788000
_diffrn_orient_matrix_UB_12      -0.0526537000
_diffrn_orient_matrix_UB_13      -0.0000306000
_diffrn_orient_matrix_UB_21      0.0026588000
_diffrn_orient_matrix_UB_22      -0.0126745000
_diffrn_orient_matrix_UB_23      0.0336551000
_diffrn_orient_matrix_UB_31      -0.0598725000
_diffrn_orient_matrix_UB_32      0.0331264000
_diffrn_orient_matrix_UB_33      0.0020793000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.810
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            28341
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.810
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.724
_diffrn_reflns_theta_min         3.308
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.704
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92537
_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            'lustrous dark red'
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_description       block
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.217
_exptl_crystal_size_min          0.127
_refine_diff_density_max         1.186
_refine_diff_density_min         -1.079
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         12829
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0308
_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/[\s^2^(Fo^2^)+6.8192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0580
_refine_ls_wR_factor_ref         0.0614
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11075
_reflns_number_total             12829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01617a2.cif
_cod_data_source_block           '[10b]+'
_cod_depositor_comments
'Adding full bibliography for 7704524--7704531.cif.'
_cod_database_code               7704527
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C54  H58  B1  N8  O2  F6  P2  W1  Pt1  '
_chemical_oxdiff_usercomment     'Vap. Diff, 5 degC, MeCN/Et2O'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.63
_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
 B1-H1
 1.15 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C11(H11), C16(H16), C20(H20), C21(H21), C27(H27), C30(H30), C36(H36),
 C37(H37), 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.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), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C)
;
_shelx_res_checksum              45166
_ins_header
;
TITL LB020_scale in P1 
REM P1 (#1 in standard setting)
CELL 0.71073  11.670112  11.729101  21.371119  79.8568  86.5053  75.0209
ZERR    2.00   0.000258   0.000358   0.000658   0.0026   0.0021   0.0023
LATT -1
SFAC C H B N O F P W Pt
UNIT 108.00 116.00 2.00 16.00 4.00 12.00 4.00 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 1.118
_oxdiff_exptl_absorpt_empirical_full_min 0.918