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_7704531
_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         'C44 H46 B Br Mo N6 O2 P2 Pt'
_chemical_formula_sum            'C44 H46 B Br Mo N6 O2 P2 Pt'
_chemical_formula_weight         1134.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                90
_cell_angle_beta                 94.581(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   42.7794(12)
_cell_length_b                   10.3970(3)
_cell_length_c                   20.4764(7)
_cell_measurement_reflns_used    12738
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.4270
_cell_measurement_theta_min      3.7310
_cell_volume                     9078.3(5)
_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 5.1872
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.842
_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    -13.00  84.50   0.75  103.58    --   10.91  37.00 -90.00  130
  2  \w    -30.00  90.00   0.75  103.58    --   10.91  19.00-150.00  160
  3  \w    -39.00 -12.00   0.75  103.58    --  -10.52  57.00 150.00   36
;
_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      0.0164389000
_diffrn_orient_matrix_UB_12      0.0008106000
_diffrn_orient_matrix_UB_13      -0.0025707000
_diffrn_orient_matrix_UB_21      -0.0023853000
_diffrn_orient_matrix_UB_22      0.0293827000
_diffrn_orient_matrix_UB_23      -0.0312631000
_diffrn_orient_matrix_UB_31      0.0009099000
_diffrn_orient_matrix_UB_32      0.0615478000
_diffrn_orient_matrix_UB_33      0.0149422000
_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  0.0382
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.842
_diffrn_reflns_limit_h_max       59
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            31105
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.842
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.737
_diffrn_reflns_theta_min         3.360
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.348
_exptl_absorpt_correction_T_max  0.790
_exptl_absorpt_correction_T_min  0.475
_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    1.660
_exptl_crystal_description       plate
_exptl_crystal_F_000             4464
_exptl_crystal_size_max          0.268
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.067
_refine_diff_density_max         1.726
_refine_diff_density_min         -1.071
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         10894
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0178P)^2^+116.5511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0929
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9093
_reflns_number_total             10894
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01617a2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7704524--7704531.cif.'
_cod_database_code               7704531
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula
'C55  H46  B1  N6  O2  P2  Br1  Mo1  Pt1  Cl1'
_chemical_oxdiff_usercomment     'DCM slow evap, 25 degC'
_reflns_odcompleteness_completeness 99.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Restrained distances
 B1-H1
 1.15 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C35(H35A,H35B)
3.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C2(H2), C55(H55), C34(H34), C4(H4), C6(H6), C21(H21), C11(H11),
 C51(H51), C25(H25), C33(H33), C22(H22), C32(H32), C53(H53), C52(H52), C54(H54),
  C01J(H01J), C44(H44), C24(H24), C23(H23)
3.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C18(H18A,H18B,H18C), C14(H14A,H14B,H14C), C13(H13A,H13B,
 H13C), C26(H26A,H26B,H26C), C8(H8A,H8B,H8C)
;
_smtbx_masks_special_details
'Refinement was complicated by a region of diffuse solvent which could not be adaquately modelled and so a solvent mask was invoked.The algorithm determined that 116 electrons were present per solvent accessible void, which corresponds well to two molecules of chloroform (216 electrons) per unit cell.The crystal strcture is presented exclusively of this solvent.'
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              63105
_shelx_fab_checksum              7257
_ins_header
;
TITL LB024_FaceMoFix in C2/c 
REM C2/c (#15 in standard setting)
CELL 0.71073  42.779419  10.396998  20.476442  90.0000  94.5811  90.0000
ZERR    7.00   0.001214   0.000309   0.000708   0.0000   0.0029   0.0000
LATT  7
SYMM -x, y,-z+1/2 
SFAC C H B N O P Cl Br Mo Pt
UNIT 385.00 322.00 7.00 42.00 14.00 14.00 7.00 7.00 7.00 7.00
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 1.088
_oxdiff_exptl_absorpt_empirical_full_min 0.932