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_7710817
_publ_section_title
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 Heterobimetallic \m2-halocarbyne complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01558G
_journal_year                    2022
_chemical_formula_moiety         'C16 H22 B Cl3 N6 W'
_chemical_formula_sum            'C16 H22 B Cl3 N6 W'
_chemical_formula_weight         599.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-09-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2022-05-15 deposited with the CCDC.	2022-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2810(4)
_cell_length_b                   12.8355(3)
_cell_length_c                   13.3658(3)
_cell_measurement_reflns_used    9396
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.5040
_cell_measurement_theta_min      4.7370
_cell_volume                     2793.12(11)
_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      150.00(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 0.888
_diffrn_measurement_details
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List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -29.00  60.00   1.00    1.00    --   37.06 -19.00-120.00   89
  2  \w     21.00 104.00   1.00    1.00    --   37.06  57.00  90.00   83
  3  \w      3.00  76.00   1.00    1.00    --   37.06 -99.00 -90.00   73
  4  \w     31.00  90.00   1.00    1.00    --   37.06-125.00 150.00   59
  5  \w    -10.00  61.00   1.00    1.00    --   37.06 -19.00  90.00   71
  6  \w     19.00  82.00   1.00    1.00    --   37.06  38.00 -90.00   63
  7  \w     20.00 104.00   1.00    1.00    --   37.06  57.00  30.00   84
  8  \w     52.00 110.00   1.00    3.48    --  111.00 -95.00 120.00   58
  9  \w     45.00 118.00   1.00    3.48    --  111.00 -30.00-120.00   73
 10  \w     46.00 149.00   1.00    3.48    --  111.00 -15.00  30.00  103
 11  \w     85.00 131.00   1.00    3.48    --  111.00  77.00  60.00   46
 12  \w    147.00 174.00   1.00    3.48    --  111.00  77.00  60.00   27
 13  \w     45.00 129.00   1.00    3.48    --  111.00 -61.00 -60.00   84
 14  \w     42.00 132.00   1.00    3.48    --  111.00 -30.00 150.00   90
 15  \w     49.00 109.00   1.00    3.48    --  111.00 -95.00 -90.00   60
 16  \w     56.00 119.00   1.00    3.48    --  111.00 -45.00  90.00   63
 17  \w     94.00 164.00   1.00    3.48    --  111.00  45.00  30.00   70
 18  \w     78.00 113.00   1.00    3.48    --  111.00-111.00  30.00   35
 19  \w     43.00 109.00   1.00    3.48    --  111.00 -45.00  30.00   66
 20  \w    108.00 138.00   1.00    3.48    --  111.00 -77.00-180.00   30
 21  \w     57.00 102.00   1.00    3.48    --  111.00 -77.00-180.00   45
;
_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      -0.0247585000
_diffrn_orient_matrix_UB_12      0.0279104000
_diffrn_orient_matrix_UB_13      0.1079599000
_diffrn_orient_matrix_UB_21      0.0590557000
_diffrn_orient_matrix_UB_22      -0.0838404000
_diffrn_orient_matrix_UB_23      0.0401374000
_diffrn_orient_matrix_UB_31      0.0697777000
_diffrn_orient_matrix_UB_32      0.0810633000
_diffrn_orient_matrix_UB_33      0.0044173000
_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  0.0462
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.888
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17210
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         85.151
_diffrn_reflns_theta_min         4.280
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.390
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65573
_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 blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       plate
_exptl_crystal_F_000             1160
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2, n-hexane'
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.049
_refine_diff_density_max         1.949
_refine_diff_density_min         -1.105
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         2930
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0828P)^2^+1.3456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1116
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2742
_reflns_number_total             2930
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01558g2.cif
_cod_data_source_block           co59_co_wcbr_phicl2_blue_scale
_cod_original_cell_volume        2793.09(11)
_cod_database_code               7710817
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C16 H22 B1 Br1 Cl2 N6 W1'
_chemical_oxdiff_usercomment     'DCM hexane'
_reflns_odcompleteness_completeness 98.23
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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. Others
 Fixed Sof: H6A(0.5) H6B(0.5) H6C(0.5) H2A(0.5) H2B(0.5) H2C(0.5)
3.a Ternary CH refined with riding coordinates:
 B1(H1)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C9(H9)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C2(H2A,H2B,H2C), C11(H11A,H11B,H11C), C7(H7A,H7B,H7C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 212 electrons were 
found in a volume of 928 ^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[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              74126
_shelx_fab_checksum              56586
_ins_header
;
TITL CO_WCBr_PhICl2_blue_scale in Pna2(1) 
REM Pna2(1) (#33, found as Pc2(1)n in cab setting)
CELL 1.54184  16.280954  12.835485  13.365755  90.0000  90.0000  90.0000
ZERR    6.00   0.000410   0.000276   0.000298   0.0000   0.0000   0.0000
LATT -1
SYMM -x,-y, z+1/2 
SYMM  x+1/2,-y+1/2, z 
SYMM -x+1/2, y+1/2, z+1/2 
SFAC C H B N Cl Br W
UNIT 96.00 132.00 6.00 36.00 12.00 6.00 6.00
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 1.381
_oxdiff_exptl_absorpt_empirical_full_min 0.798