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_7704526
_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         'C46 H53 B2 N10 O2 P Pt W, C H Cl3'
_chemical_formula_sum            'C47 H54 B2 Cl3 N10 O2 P Pt W'
_chemical_formula_weight         1328.88
_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             2020-04-18
_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                103.794(4)
_cell_angle_beta                 102.422(4)
_cell_angle_gamma                106.487(5)
_cell_formula_units_Z            2
_cell_length_a                   10.1322(6)
_cell_length_b                   14.7017(8)
_cell_length_c                   19.3416(7)
_cell_measurement_reflns_used    5878
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.7550
_cell_measurement_theta_min      4.6570
_cell_volume                     2556.3(3)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  66.00   1.00    8.60    --   36.34 -99.00  30.00   51
  2  \w      9.00 100.00   1.00    8.60    --   36.34  19.00 -30.00   91
  3  \w     41.00 101.00   1.00    8.60    --   36.34  57.00 -30.00   60
  4  \w     11.00  75.00   1.00    8.60    --   36.34 -99.00 -90.00   64
  5  \w     29.00  90.00   1.00    8.60    --   36.34-125.00-180.00   61
  6  \w    -33.00  55.00   1.00    8.60    --   36.34 -38.00 120.00   88
  7  \w     49.00 101.00   1.00    8.60    --   36.34  19.00-120.00   52
  8  \w     14.00  41.00   1.00    8.60    --   36.34  19.00-120.00   27
  9  \w    -30.00  53.00   1.00    8.60    --   36.34 -57.00  30.00   83
 10  \w    116.00 176.00   1.00   34.38    --  109.99 111.00-150.00   60
 11  \w     57.00 109.00   1.00   34.38    --  109.99-111.00  60.00   52
 12  \w     70.00 127.00   1.00   34.38    --  109.99 -45.00 120.00   57
 13  \w     62.00 106.00   1.00   34.38    --  109.99 -95.00-150.00   44
 14  \w     43.00 123.00   1.00   34.38    --  109.99 -45.00 -60.00   80
 15  \w    103.00 177.00   1.00   34.38    --  109.99  77.00 -90.00   74
 16  \w     52.00 111.00   1.00   34.38    --  109.99 -77.00 -90.00   59
 17  \w     43.00  68.00   1.00   34.38    --  109.99 -45.00 120.00   25
 18  \w     89.00 126.00   1.00   34.38    --  109.99 -61.00 150.00   37
 19  \w     41.00 122.00   1.00   34.38    --  109.99 -30.00-150.00   81
 20  \w    104.00 145.00   1.00   34.38    --  109.99 111.00-120.00   41
 21  \w     49.00  76.00   1.00   34.38    --  109.99 -61.00 150.00   27
 22  \w     47.00 109.00   1.00   34.38    --  109.99-111.00 150.00   62
 23  \w     45.00 178.00   1.00   34.38    --  109.99   0.00  60.00  133
;
_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      0.0698634000
_diffrn_orient_matrix_UB_12      -0.0797578000
_diffrn_orient_matrix_UB_13      -0.0172293000
_diffrn_orient_matrix_UB_21      0.0149377000
_diffrn_orient_matrix_UB_22      0.0239014000
_diffrn_orient_matrix_UB_23      -0.0718933000
_diffrn_orient_matrix_UB_31      0.1503095000
_diffrn_orient_matrix_UB_32      0.0798137000
_diffrn_orient_matrix_UB_33      0.0440937000
_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  0.0456
_diffrn_reflns_av_unetI/netI     0.0912
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15942
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.246
_diffrn_reflns_theta_min         4.664
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.265
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60396
_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    1.726
_exptl_crystal_description       plate
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.093
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.043
_refine_diff_density_max         2.080
_refine_diff_density_min         -2.120
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         9298
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0395P)^2^+7.5238P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1274
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6912
_reflns_number_total             9298
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01617a2.cif
_cod_data_source_block           11
_cod_depositor_comments
'Adding full bibliography for 7704524--7704531.cif.'
_cod_original_cell_volume        2556.3(2)
_cod_database_code               7704526
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C46 H53 B2 N10 O2 P1 Pt1 W1'
_chemical_oxdiff_usercomment     'CHCl3/n-hex vap. diff @0 degC'
_reflns_odcompleteness_completeness 99.24
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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
 B2-H2B
 1.15 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C70(H70)
3.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C62(H62), C37(H37), C45(H45), C52(H52), C61(H61), C17(H17),
 C65(H65), C51(H51), C55(H55), C43(H43), C53(H53), C22(H22), C41(H41), C64(H64),
  C44(H44), C12(H12), C42(H42), C54(H54), C63(H63)
3.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C15(H15A,H15B,H15C), C35(H35A,H35B,H35C), C20(H20A,H20B,
 H20C), C10(H10A,H10B,H10C), C39(H39A,H39B,H39C), C34(H34A,H34B,H34C), C19(H19A,
 H19B,H19C), C24(H24A,H24B,H24C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              47521
_ins_header
;
TITL LB010_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  10.132171  14.701748  19.341631 103.7940 102.4218 106.4867
ZERR    2.00   0.000588   0.000847   0.000657   0.0039   0.0040   0.0051
LATT  1
SFAC C H B N O P W Pt
UNIT 92.00 106.00 4.00 20.00 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 1.568
_oxdiff_exptl_absorpt_empirical_full_min 0.499