A heterobimetallic cumulenic μ-carbido complex.
Hill, Anthony F.; Watson, Lachlan J.; Chemical communications (Cambridge, England) 56 (2020) 2356–2359; doi:10.1039/c9cc08172k

data_7125781
_publ_section_title
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 A heterobimetallic cumulenic \m-carbido complex.
;
_journal_issue                   15
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2356
_journal_page_last               2359
_journal_paper_doi               10.1039/c9cc08172k
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C24 H27 B N7 O4 Re W, C H2 Cl2'
_chemical_formula_sum            'C25 H29 B Cl2 N7 O4 Re W'
_chemical_formula_weight         943.31
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Light-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-13 deposited with the CCDC.	2020-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.221(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0943(4)
_cell_length_b                   21.8669(10)
_cell_length_c                   17.3220(7)
_cell_measurement_reflns_used    9717
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.2490
_cell_measurement_theta_min      3.8470
_cell_volume                     3053.2(2)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -42.00  44.00   1.00  180.00    --   11.46 -77.00 150.00   86
  2  \w    -17.00  84.00   1.00  180.00    --   11.46  57.00 -60.00  101
  3  \w    -16.00  34.00   1.00  180.00    --   11.46  77.00  30.00   50
  4  \w     -7.00  79.00   1.00  180.00    --   11.46  37.00  90.00   86
  5  \w     -5.00  20.00   1.00  180.00    --   11.46 -99.00  60.00   25
  6  \w    -42.00 -14.00   1.00  180.00    --   11.46 -77.00-120.00   28
  7  \w     39.00  64.00   1.00  180.00    --   11.46-178.00 120.00   25
;
_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      0.0123139000
_diffrn_orient_matrix_UB_12      -0.0212671000
_diffrn_orient_matrix_UB_13      0.0309295000
_diffrn_orient_matrix_UB_21      0.0579735000
_diffrn_orient_matrix_UB_22      0.0201451000
_diffrn_orient_matrix_UB_23      0.0198316000
_diffrn_orient_matrix_UB_31      -0.0650146000
_diffrn_orient_matrix_UB_32      0.0139325000
_diffrn_orient_matrix_UB_33      0.0184800000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_unetI/netI     0.0578
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31774
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         3.273
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.944
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85282
_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 pale yellow'
_exptl_crystal_density_diffrn    2.052
_exptl_crystal_description       plate
_exptl_crystal_F_000             1792
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane'
_exptl_crystal_size_max          0.203
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.028
_refine_diff_density_max         1.450
_refine_diff_density_min         -1.054
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         6229
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0231P)^2^+0.1200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0651
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5073
_reflns_number_total             6229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08172k3.cif
_cod_data_source_block           Compound_5C
_cod_depositor_comments
'Adding full bibliography for 7125781--7125782.cif.'
_cod_database_code               7125781
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C25 H27 B Cl2 N7 O4 Re W'
_chemical_oxdiff_usercomment     'dcm/hex liquid diff -20'
_reflns_odcompleteness_completeness 99.74
_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.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B)
2.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C22(H22), C24(H24), C7(H7), C17(H17), C21(H21), C20(H20), C12(H12)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C10(H10A,H10B,H10C), C5(H5A,H5B,H5C), C19(H19A,H19B,
 H19C), C9(H9A,H9B,H9C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              44609
_ins_header
;
TITL LJW-223-3-a_scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073   8.094264  21.866872  17.321973  90.0000  95.2214  90.0000
ZERR    4.00   0.000400   0.001042   0.000681   0.0000   0.0037   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H B N O Cl W Re
UNIT 100.00 108.00 4.00 28.00 16.00 8.00 4.00 4.00
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 1.389
_oxdiff_exptl_absorpt_empirical_full_min 0.876