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_7704529
_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
'C H Cl3, C44 H47 B2 N10 O2 P Pt0.972 S2 W0.972, 0.028(Pt1), 0.028(W1)'
_chemical_formula_sum            'C45 H48 B2 Cl3 N10 O2 P Pt S2 W'
_chemical_formula_weight         1362.93
_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                74.259(4)
_cell_angle_beta                 82.640(5)
_cell_angle_gamma                76.417(5)
_cell_formula_units_Z            2
_cell_length_a                   11.8325(10)
_cell_length_b                   12.6410(5)
_cell_length_c                   18.1325(7)
_cell_measurement_reflns_used    6546
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.6650
_cell_measurement_theta_min      4.7350
_cell_volume                     2531.4(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 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 0.996
_diffrn_measured_fraction_theta_max 0.971
_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    -31.00  18.00   1.00   10.00    --   38.31 -19.00  60.00   49
  2  \w     37.00  63.00   1.00   10.00    --   38.31  57.00  60.00   26
  3  \w     67.00 104.00   1.00   10.00    --   38.31  57.00 -90.00   37
  4  \w     40.00  69.00   1.00   10.00    --   38.31 -99.00 -30.00   29
  5  \w    -29.00   3.00   1.00   10.00    --   38.31 -44.00-117.00   32
  6  \w     35.00  75.00   1.00   10.00    --   38.31 -99.00 120.00   40
  7  \w     31.00  65.00   1.00   10.00    --   38.31  19.00   0.00   34
  8  \w     20.00  51.00   1.00   10.00    --   38.31  38.00 120.00   31
  9  \w     28.00  53.00   1.00   10.00    --   38.31 -57.00 -30.00   25
 10  \w    -29.00  35.00   1.00   10.00    --   38.31 -57.00-120.00   64
 11  \w    -18.00  17.00   1.00   10.00    --   38.31 -77.00 150.00   35
 12  \w     19.00  65.00   1.00   10.00    --   38.31 -77.00-180.00   46
 13  \w     -9.00  36.00   1.00   10.00    --   38.31 -57.00-150.00   45
 14  \w     27.00  54.00   1.00   10.00    --   38.31  57.00 -60.00   27
 15  \w     81.00 106.00   1.00   10.00    --   38.31  19.00   0.00   25
 16  \w     61.00  92.00   1.00   10.00    --   38.31-125.00-180.00   31
 17  \w     -3.00  52.00   1.00   10.00    --   38.31 -57.00  90.00   55
 18  \w     69.00  94.00   1.00   10.00    --   38.31  38.00 120.00   25
 19  \w     76.00 106.00   1.00   10.00    --   38.31   0.00  60.00   30
 20  \w     13.00  46.00   1.00   10.00    --   38.31 -57.00 -90.00   33
 21  \w    -28.00  -3.00   1.00   10.00    --   38.31 -57.00 -30.00   25
 22  \w     26.00  64.00   1.00   10.00    --   38.31 -77.00-150.00   38
 23  \w     38.00  77.00   1.00   10.00    --   38.31  38.00  30.00   39
 24  \w     32.00  59.00   1.00   10.00    --   38.31 -77.00 150.00   27
 25  \w     36.00  65.00   1.00   10.00    --   38.31 -77.00  60.00   29
 26  \w    -23.00  55.00   1.00   10.00    --   38.31   0.00  60.00   78
 27  \w    -21.00   9.00   1.00   10.00    --   38.31 -77.00-150.00   30
 28  \w      6.00  36.00   1.00   10.00    --   38.31 -99.00   0.00   30
 29  \w     47.00  72.00   1.00   10.00    --   38.31 -99.00   0.00   25
 30  \w     23.00  51.00   1.00   10.00    --   38.31  57.00 150.00   28
 31  \w     73.00  98.00   1.00   10.00    --   38.31  57.00 150.00   25
 32  \w     46.00  91.00   1.00   10.00    --   38.31-125.00 120.00   45
 33  \w     51.00  97.00   1.00   10.00    --   38.31  38.00-150.00   46
 34  \w      3.00  28.00   1.00   10.00    --   38.31 -38.00-180.00   25
 35  \w     20.00  51.00   1.00   10.00    --   38.31 -38.00 120.00   31
 36  \w     44.00  87.00   1.00   10.00    --   38.31-125.00 150.00   43
 37  \w    -17.00  12.00   1.00   10.00    --   38.31 -19.00 -30.00   29
 38  \w     21.00  48.00   1.00   10.00    --   38.31 -19.00 -30.00   27
 39  \w    100.00 131.00   1.00   12.00    --  111.00  50.00 -90.00   31
 40  \w    126.00 173.00   1.00   12.00    --  111.00  38.00 -60.00   47
 41  \w     98.00 176.00   1.00   12.00    --  111.00  50.00-120.00   78
 42  \w     53.00 104.00   1.00   12.00    --  111.00 -92.00-180.00   51
 43  \w    106.00 172.00   1.00   12.00    --  111.00  77.00 150.00   66
 44  \w    114.00 178.00   1.00   12.00    --  111.00  77.00-150.00   64
 45  \w     85.00 131.00   1.00   12.00    --  111.00 -64.00 -60.00   46
 46  \w     45.00 129.00   1.00   12.00    --  111.00 -38.00  90.00   84
 47  \w     84.00 109.00   1.00   12.00    --  111.00-111.00 150.00   25
 48  \w     46.00  84.00   1.00   12.00    --  111.00 -50.00 -90.00   38
 49  \w     44.00 106.00   1.00   12.00    --  111.00 -92.00 -60.00   62
 50  \w    140.00 176.00   1.00   12.00    --  111.00  50.00  60.00   36
 51  \w     42.00  69.00   1.00   12.00    --  111.00-111.00 150.00   27
 52  \w     55.00 107.00   1.00   12.00    --  111.00-111.00  90.00   52
 53  \w    104.00 168.00   1.00   12.00    --  111.00  77.00-180.00   64
 54  \w     80.00 107.00   1.00   12.00    --  111.00-111.00  60.00   27
 55  \w    111.00 171.00   1.00   12.00    --  111.00 111.00 120.00   60
 56  \w     44.00  97.00   1.00   12.00    --  111.00 -77.00  90.00   53
 57  \w     67.00 113.00   1.00   12.00    --  111.00 -50.00-180.00   46
 58  \w    144.00 174.00   1.00   12.00    --  111.00  50.00 -90.00   30
 59  \w     74.00 109.00   1.00   12.00    --  111.00-111.00 -90.00   35
 60  \w     74.00 122.00   1.00   12.00    --  111.00 -53.00 133.38   48
 61  \w     41.00 111.00   1.00   12.00    --  111.00 -15.00-145.07   70
;
_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      0.0595581000
_diffrn_orient_matrix_UB_12      0.0591575000
_diffrn_orient_matrix_UB_13      0.0431251000
_diffrn_orient_matrix_UB_21      0.0926175000
_diffrn_orient_matrix_UB_22      -0.1087938000
_diffrn_orient_matrix_UB_23      0.0242747000
_diffrn_orient_matrix_UB_31      0.0768179000
_diffrn_orient_matrix_UB_32      0.0378620000
_diffrn_orient_matrix_UB_33      -0.0733480000
_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  0.0523
_diffrn_reflns_av_unetI/netI     0.0890
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23660
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.722
_diffrn_reflns_theta_min         3.941
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.146
_exptl_absorpt_correction_T_max  0.756
_exptl_absorpt_correction_T_min  0.320
_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_density_diffrn    1.788
_exptl_crystal_description       plate
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.199
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.819
_refine_diff_density_min         -2.004
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         9955
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0613
_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^)+(0.0503P)^2^+28.3154P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1626
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6644
_reflns_number_total             9955
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01617a2.cif
_cod_data_source_block           13
_cod_depositor_comments
'Adding full bibliography for 7704524--7704531.cif.'
_cod_database_code               7704529
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C45 H47 O2 N10 P1Cl3 B2 S2 Pt1 W1'
_chemical_oxdiff_usercomment     'Vap diff, n-Pent into CHCl3 @ 0 deg C'
_reflns_odcompleteness_completeness 98.62
_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
 B1-H1
 1.15 with sigma of 0.02
 B2-H2A = B2-H2B
 1.15 with sigma of 0.02
3. Rigid bond restraints
 Pt1, W1, C1
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
Pt1 \\sim W1 \\sim C1: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 2A
Uanis(C15) = Uanis(C16) = Uanis(C17)
5. Others
 Sof(Pt2)=Sof(W2)=1-FVAR(1)
 Sof(Pt1)=Sof(W1)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C60(H60)
6.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C11(H11), C21(H21), C22(H22), C23(H23), C24(H24), C31(H31), C32(H32),
 C33(H33), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C51(H51), C52(H52),
  C53(H53), C54(H54), C55(H55)
6.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), C20(H20A,H20B,H20C), C25(H25A,H25B,
 H25C)
;
_shelx_res_checksum              87027
_shelx_fab_checksum              95564
_ins_header
;
TITL LB015_Faces_050Filt in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  11.832548  12.640954  18.132545  74.2589  82.6395  76.4174
ZERR    2.00   0.000962   0.000532   0.000670   0.0035   0.0047   0.0051
LATT  1
SFAC C H B N O P S Cl W Pt
UNIT 90.00 94.00 4.00 20.00 4.00 2.00 4.00 6.00 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 1.417
_oxdiff_exptl_absorpt_empirical_full_min 0.602