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_7710820
_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         'C18 H22 Au B Br Cl N6 O2 W'
_chemical_formula_sum            'C18 H22 Au B Br Cl N6 O2 W'
_chemical_formula_weight         861.40
_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
_audit_creation_date             2020-09-02
_audit_creation_method
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Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_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                 107.856(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.3829(4)
_cell_length_b                   10.99020(10)
_cell_length_c                   19.8684(3)
_cell_measurement_reflns_used    19131
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      71.9460
_cell_measurement_theta_min      4.4030
_cell_volume                     5275.57(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_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    -53.00  31.00   1.00    1.00    --  -36.03  57.00-180.00   84
  2  \w   -107.00  -7.00   1.00    1.00    --  -36.03 -19.00   4.00  100
  3  \w   -103.00 -19.00   1.00    1.00    --  -36.03 -57.00 -60.00   84
  4  \w     23.00  89.00   1.00    1.00    --   36.03-125.00  60.00   66
  5  \w     23.00  89.00   1.00    1.00    --   36.03-125.00 -90.00   66
  6  \w     57.00 151.00   1.00    2.00    --  107.33 178.00 120.00   94
  7  \w     41.00 112.00   1.00    2.00    --  107.33-111.00-150.00   71
  8  \w     40.00 131.00   1.00    2.00    --  107.33 -77.00-150.00   91
  9  \w     40.00 121.00   1.00    2.00    --  107.33 -45.00  60.00   81
 10  \w    101.00 172.00   1.00    2.00    --  107.33  77.00-150.00   71
 11  \w     39.00 121.00   1.00    2.00    --  107.33 -45.00-150.00   82
 12  \w     38.00 175.00   1.00    2.00    --  107.33   0.00   0.00  137
 13  \w    119.00 163.00   1.00    2.00    --  107.33 111.00 120.00   44
 14  \w     59.00 115.00   1.00    2.00    --  107.33 -30.00 120.00   56
 15  \w     38.00 110.00   1.00    2.00    --  107.33 -95.00  60.00   72
;
_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      0.0000393000
_diffrn_orient_matrix_UB_12      -0.0968771000
_diffrn_orient_matrix_UB_13      -0.0560220000
_diffrn_orient_matrix_UB_21      -0.0161365000
_diffrn_orient_matrix_UB_22      0.0980666000
_diffrn_orient_matrix_UB_23      -0.0581571000
_diffrn_orient_matrix_UB_31      0.0616981000
_diffrn_orient_matrix_UB_32      0.0255668000
_diffrn_orient_matrix_UB_33      0.0105771000
_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  0.0499
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31402
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.030
_diffrn_reflns_theta_min         4.420
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    21.163
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    2.169
_exptl_crystal_description       plate
_exptl_crystal_F_000             3184
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2, n-hexane'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.053
_refine_diff_density_max         1.811
_refine_diff_density_min         -1.913
_refine_diff_density_rms         0.278
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         10375
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0656P)^2^+80.3361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1329
_refine_ls_wR_factor_ref         0.1366
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9259
_reflns_number_total             10375
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01558g2.cif
_cod_data_source_block           co24_wcbr_aucl_scale
_cod_database_code               7710820
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C29 H43 B1 N6 O2 Si1 Cl1 W1 Au1'
_chemical_oxdiff_usercomment     'DCM hex'
_shelx_estimated_absorpt_t_max   0.400
_shelx_estimated_absorpt_t_min   0.080
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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. Uiso/Uaniso restraints and constraints
Uanis(O2A) = Uanis(O2)
Uanis(B1) = Uanis(B1A)
Uanis(N3) = Uanis(N1)
3.a Ternary CH refined with riding coordinates:
 B1(H1)
3.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C11A(H11A), C6A(H6A), C11(H11), C16A(H16A), C6(H6)
3.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C18(H18A,H18B,H18C), C13A(H13D,H13E,H13F), C9A(H9AA,H9AB,
 H9AC), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C14A(H14D,H14E,H14F), C4(H4A,
 H4B,H4C), C18A(H18D,H18E,H18F), C4A(H4AA,H4AB,H4AC), C8A(H8AA,H8AB,H8AC),
 C8(H8A,H8B,H8C)
;
_smtbx_masks_special_details
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A solvent mask was calculated and 228 electrons were 
found in a volume of 704 A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.5[C6H14] per Asymmetric Unit 
which account for 200 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              16363
_shelx_fab_checksum              39612
_ins_header
;
TITL CO24_scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 1.54184  25.374190  10.989645  19.868488  90.0000 107.8374  90.0000
ZERR    7.00   0.000340   0.000135   0.000299   0.0000   0.0015   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H B N O Si Cl W Au
UNIT 203.00 301.00 7.00 42.00 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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.877
_oxdiff_exptl_absorpt_empirical_full_min 0.575