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_7704525
_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 H45 B N8 O2 P Pt W, 2(C H Cl3), F6 P'
_chemical_formula_sum            'C48 H47 B Cl6 F6 N8 O2 P2 Pt W'
_chemical_formula_weight         1546.32
_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                84.892(2)
_cell_angle_beta                 78.583(2)
_cell_angle_gamma                85.769(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5287(2)
_cell_length_b                   16.3575(4)
_cell_length_c                   18.2918(2)
_cell_measurement_reflns_used    8793
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.3100
_cell_measurement_theta_min      4.7450
_cell_volume                     2778.94(10)
_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 2018/2 (Sheldrick, 2018)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.969
_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    -73.00  27.00   1.00    1.19    --  -37.05   0.00  30.00  100
  2  \w     28.00  90.00   1.00    1.19    --   37.05-125.00 150.00   62
  3  \w    -13.00  54.00   1.00    1.19    --   37.05 -57.00   0.00   67
  4  \w     28.00  66.00   1.00    1.19    --   37.05 -19.00  60.00   38
  5  \w    -25.00  18.00   1.00    1.19    --   37.05 -19.00  60.00   43
  6  \w      7.00  70.00   1.00    1.19    --   37.05 -99.00 -30.00   63
  7  \w      9.00 108.00   1.00    1.19    --   37.05  19.00 -90.00   99
  8  \w     35.00  76.00   1.00    1.19    --   37.05-125.00 -90.00   41
  9  \w     44.00 109.00   1.00    4.76    --  111.00-111.00 -90.00   65
 10  \w     41.00 109.00   1.00    4.76    --  111.00-111.00  30.00   68
 11  \w     97.00 178.00   1.00    4.76    --  111.00  25.00  90.00   81
 12  \w     47.00 109.00   1.00    4.76    --  111.00-111.00 -30.00   62
 13  \w     43.00 128.00   1.00    4.76    --  111.00 -38.00  30.00   85
 14  \w     43.00 128.00   1.00    4.76    --  111.00 -50.00-120.00   85
 15  \w     42.00 114.00   1.00    4.76    --  111.00 -38.00 120.00   72
 16  \w    132.00 174.00   1.00    4.76    --  111.00  77.00  30.00   42
 17  \w     42.00  96.00   1.00    4.76    --  111.00 -38.00 -30.00   54
 18  \w     49.00  99.00   1.00    4.76    --  111.00 -92.00-180.00   50
 19  \w     52.00 132.00   1.00    4.76    --  111.00 -77.00  30.00   80
 20  \w     81.00 109.00   1.00    4.76    --  111.00-111.00 150.00   28
 21  \w     63.00 178.00   1.00    4.76    --  111.00   0.00-150.00  115
;
_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      0.0106110000
_diffrn_orient_matrix_UB_12      0.0939995000
_diffrn_orient_matrix_UB_13      -0.0099073000
_diffrn_orient_matrix_UB_21      -0.1497857000
_diffrn_orient_matrix_UB_22      0.0098309000
_diffrn_orient_matrix_UB_23      -0.0206071000
_diffrn_orient_matrix_UB_31      -0.0689000000
_diffrn_orient_matrix_UB_32      0.0061680000
_diffrn_orient_matrix_UB_33      0.0830828000
_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  0.0427
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18617
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.935
_diffrn_reflns_theta_min         3.811
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.182
_exptl_absorpt_correction_T_max  0.696
_exptl_absorpt_correction_T_min  0.199
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.36a (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.848
_exptl_crystal_description       plate
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.188
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.036
_refine_diff_density_max         1.427
_refine_diff_density_min         -2.374
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         10934
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0663P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1252
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9217
_reflns_number_total             10934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01617a2.cif
_cod_data_source_block           '[10a]+'
_cod_depositor_comments
'Adding full bibliography for 7704524--7704531.cif.'
_cod_database_code               7704525
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C45H44BO2Cl6F6N8P2Pt1W1
_chemical_oxdiff_usercomment     'Vap. diff. CDCl3/Hex, -20 degC'
_reflns_odcompleteness_completeness 99.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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 Ternary CH refined with riding coordinates:
 C60(H60), C61(H61)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C11(H11), C16(H16), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26),
 C27(H27), C28(H28), C29(H29), 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)
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)
;
_shelx_res_checksum              92754
_ins_header
;
TITL LB019_Rint033abs in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184   9.528668  16.357473  18.291797  84.8920  78.5833  85.7688
ZERR    2.00   0.000219   0.000423   0.000237   0.0016   0.0016   0.0020
LATT  1
SFAC C H B N O F P Cl W Pt
UNIT 90.00 88.00 2.00 16.00 4.00 12.00 4.00 12.00 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 2.231
_oxdiff_exptl_absorpt_empirical_full_min 0.579