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_7704530
_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         'C41 H47 B N7 O2 P Pt S2 W'
_chemical_formula_sum            'C41 H47 B N7 O2 P Pt S2 W'
_chemical_formula_weight         1154.69
_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                76.4350(10)
_cell_angle_beta                 89.1410(10)
_cell_angle_gamma                82.5190(10)
_cell_formula_units_Z            2
_cell_length_a                   12.5263(2)
_cell_length_b                   12.9390(2)
_cell_length_c                   13.8769(2)
_cell_measurement_reflns_used    21718
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.5970
_cell_measurement_theta_min      4.8630
_cell_volume                     2167.50(6)
_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 0.999
_diffrn_measured_fraction_theta_max 0.988
_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     27.00  90.00   1.00    1.41    --   36.95-125.00 -30.00   63
  2  \w     20.00 104.00   1.00    1.41    --   36.95  57.00-120.00   84
  3  \w     18.00 106.00   1.00    1.41    --   36.95  38.00-150.00   88
  4  \w    -30.00  54.00   1.00    1.41    --   36.95 -57.00 -60.00   84
  5  \w    -21.00  64.00   1.00    1.41    --   36.95 -77.00  30.00   85
  6  \w     18.00 106.00   1.00    1.41    --   36.95  38.00 120.00   88
  7  \w      5.00  31.00   1.00    1.41    --   36.95  87.00 155.31   26
  8  \w     42.00 130.00   1.00    5.62    --  111.00 -38.00  30.00   88
  9  \w    103.00 178.00   1.00    5.62    --  111.00  77.00 -30.00   75
 10  \w     44.00 131.00   1.00    5.62    --  111.00 -64.00 -60.00   87
 11  \w     41.00 109.00   1.00    5.62    --  111.00-111.00  90.00   68
 12  \w     42.00 130.00   1.00    5.62    --  111.00 -38.00-120.00   88
 13  \w     92.00 178.00   1.00    5.62    --  111.00  38.00  30.00   86
 14  \w     94.00 178.00   1.00    5.62    --  111.00  52.00-139.00   84
 15  \w     41.00 109.00   1.00    5.62    --  111.00-111.00-150.00   68
 16  \w     44.00 131.00   1.00    5.62    --  111.00 -64.00-150.00   87
 17  \w     41.00 109.00   1.00    5.62    --  111.00-111.00 -60.00   68
 18  \w     43.00 138.00   1.00    5.62    --  111.00 -77.00  90.00   95
 19  \w     41.00 109.00   1.00    5.62    --  111.00-111.00   0.00   68
 20  \w     65.00 178.00   1.00    5.62    --  111.00  12.00 -30.00  113
 21  \w    -54.00  30.00   1.00    1.41    --  -36.95  57.00-120.00   84
 22  \w      8.00 108.00   1.00    1.41    --   36.95  19.00  30.00  100
 23  \w      3.00  29.00   1.00    1.41    --   36.95  90.00  57.77   26
 24  \w      4.00  30.00   1.00    1.41    --   36.95  89.00   8.83   26
 25  \w    -30.00  54.00   1.00    1.41    --   36.95 -57.00  90.00   84
 26  \w      7.00  36.00   1.00    1.41    --   36.95  82.00 -37.49   29
 27  \w     91.00 178.00   1.00    5.62    --  111.00  64.00-120.00   87
 28  \w     92.00 178.00   1.00    5.62    --  111.00  38.00-150.00   86
 29  \w     86.00 178.00   1.00    5.62    --  111.00  25.00   0.00   92
 30  \w     92.00 178.00   1.00    5.62    --  111.00  38.00  60.00   86
 31  \w     94.00 178.00   1.00    5.62    --  111.00  50.00 -60.00   84
 32  \w     92.00 178.00   1.00    5.62    --  111.00  38.00 120.00   86
 33  \w     91.00 178.00   1.00    5.62    --  111.00  64.00  60.00   87
 34  \w     94.00 178.00   1.00    5.62    --  111.00  50.00   0.00   84
 35  \w     91.00 178.00   1.00    5.62    --  111.00  64.00 -90.00   87
 36  \w     92.00 178.00   1.00    5.62    --  111.00  38.00-180.00   86
 37  \w     27.00  90.00   1.00    1.41    --   36.95-125.00-180.00   63
 38  \w     18.00 106.00   1.00    1.41    --   36.95  38.00  90.00   88
 39  \w      5.00  31.00   1.00    1.41    --   36.95  87.00 -94.35   26
 40  \w     15.00 104.00   1.00    1.41    --   36.95  68.00 -54.40   89
 41  \w     10.00  42.00   1.00    1.41    --   36.95  77.00-164.94   32
 42  \w      5.00  31.00   1.00    1.41    --   36.95  87.00  92.69   26
 43  \w     94.00 178.00   1.00    5.62    --  111.00  50.00-120.00   84
 44  \w     94.00 178.00   1.00    5.62    --  111.00  50.00-180.00   84
 45  \w     86.00 178.00   1.00    5.62    --  111.00  73.00 109.88   92
 46  \w     91.00 178.00   1.00    5.62    --  111.00  64.00 -60.00   87
 47  \w     92.00 178.00   1.00    5.62    --  111.00  38.00   0.00   86
 48  \w     94.00 178.00   1.00    5.62    --  111.00  50.00  30.00   84
 49  \w     94.00 178.00   1.00    5.62    --  111.00  50.00 150.00   84
;
_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      -0.0448117000
_diffrn_orient_matrix_UB_12      0.0809836000
_diffrn_orient_matrix_UB_13      0.0608351000
_diffrn_orient_matrix_UB_21      -0.1145649000
_diffrn_orient_matrix_UB_22      -0.0011832000
_diffrn_orient_matrix_UB_23      -0.0382206000
_diffrn_orient_matrix_UB_31      -0.0160396000
_diffrn_orient_matrix_UB_32      -0.0932785000
_diffrn_orient_matrix_UB_33      0.0887906000
_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  0.0382
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39525
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.760
_diffrn_reflns_theta_min         3.544
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.373
_exptl_absorpt_correction_T_max  0.743
_exptl_absorpt_correction_T_min  0.315
_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 yellow'
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_description       plate
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.026
_refine_diff_density_max         1.341
_refine_diff_density_min         -0.998
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         8662
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0468P)^2^+0.6870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7905
_reflns_number_total             8662
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01617a2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7704524--7704531.cif.'
_cod_database_code               7704530
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C41 H47 B1 N7 O2 P1 Pt1 S2 W1'
_chemical_oxdiff_usercomment     'CH/MeOH vap diff, 5 degC'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C53(H53A,H53B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C11(H11), C16(H16), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25),
 C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C41(H41), C42(H42), C43(H43),
  C44(H44), C45(H45)
2.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), C52(H52A,H52B,H52C), C54(H54A,H54B,
 H54C)
;
_shelx_res_checksum              97103
_ins_header
;
TITL LB028_Rint016Faces in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  12.526276  12.938982  13.876893  76.4350  89.1406  82.5192
ZERR    2.00   0.000207   0.000203   0.000218   0.0013   0.0013   0.0013
LATT  1
SFAC C H B N O P S W Pt
UNIT 82.00 94.00 2.00 14.00 4.00 2.00 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 1.365
_oxdiff_exptl_absorpt_empirical_full_min 0.730