Heterobimetallic μ2-halocarbyne complexes
Burt, Liam K.; Dewhurst, Rian D.; Hill, Anthony F.; Kong, Richard Y.; Nahon, Emily E.; Onn, Chee S.; Dalton Transactions  (2022) –; doi:10.1039/D2DT01558G

data_7710818
_publ_section_title
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 Heterobimetallic \m2-halocarbyne complexes
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01558G
_journal_year                    2022
_chemical_formula_moiety         'C15 H22 B Cl3 N6 W'
_chemical_formula_sum            'C15 H22 B Cl3 N6 W'
_chemical_formula_weight         587.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
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_audit_update_record
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2022-05-15 deposited with the CCDC.	2022-07-27 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 99.903(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.0658(3)
_cell_length_b                   14.0050(6)
_cell_length_c                   9.0433(3)
_cell_measurement_reflns_used    2554
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.3820
_cell_measurement_theta_min      4.2750
_cell_volume                     1006.32(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_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 0.847
_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     -1.00  83.00   1.00    4.64    --   15.42  57.00 -90.00   84
  2  \w      1.00  72.00   1.00    4.64    --   15.42  77.00 -30.00   71
  3  \w     14.00  60.00   1.00    4.64    --   15.42  19.00-120.00   46
;
_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      -0.0218636000
_diffrn_orient_matrix_UB_12      0.0022186000
_diffrn_orient_matrix_UB_13      -0.0793322000
_diffrn_orient_matrix_UB_21      0.0027697000
_diffrn_orient_matrix_UB_22      -0.0505393000
_diffrn_orient_matrix_UB_23      -0.0038379000
_diffrn_orient_matrix_UB_31      -0.0865266000
_diffrn_orient_matrix_UB_32      -0.0021348000
_diffrn_orient_matrix_UB_33      0.0057413000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.847
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4499
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.847
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.124
_diffrn_reflns_theta_min         3.450
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.150
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.939
_exptl_crystal_description       plate
_exptl_crystal_F_000             568
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2, n-hexane'
_exptl_crystal_size_max          0.255
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.062
_refine_diff_density_max         1.532
_refine_diff_density_min         -1.052
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         2381
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0235P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0684
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2199
_reflns_number_total             2381
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01558g2.cif
_cod_data_source_block           co59a_xrdsn
_cod_database_code               7710818
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C15 H22 B1 N6 W1 Cl3'
_chemical_oxdiff_usercomment     'DCM hexane, clearly different band from blue'
_reflns_odcompleteness_completeness 99.03
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  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. Uiso/Uaniso restraints and constraints
Uanis(C10) = Uanis(C9) = Uanis(C8) = Uanis(C7) = Uanis(C6)
4. Others
 Fixed Sof: H6A(0.5) H6B(0.5) H6C(0.5) H10A(0.5) H10B(0.5) H10C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C3(H3)
5.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C10(H10A,H10B,H10C)
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_shelx_res_checksum              94876
_ins_header
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TITL CO_WSeHg_AuCl_yellow - actually_scale in P2(1) 
REM P2(1) (#4 in standard setting)
CELL 0.71073   8.065768  14.005001   9.043294  90.0000  99.9034  90.0000
ZERR    2.00   0.000258   0.000570   0.000317   0.0000   0.0033   0.0000
LATT -1
SYMM -x, y+1/2,-z 
SFAC C H B N Cl W
UNIT 30.00 44.00 2.00 12.00 6.00 2.00
TREF
HKLF 4
END
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_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 1.394
_oxdiff_exptl_absorpt_empirical_full_min 0.789