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_7710826
_publ_section_title
;
 Heterobimetallic \m2-halocarbyne complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01558G
_journal_year                    2022
_chemical_formula_moiety         'C18 H22 B Br N6 O2 W'
_chemical_formula_sum            'C18 H22 B Br N6 O2 W'
_chemical_formula_weight         628.98
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-15
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_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                   20.2626(3)
_cell_length_b                   13.7288(3)
_cell_length_c                   7.9566(2)
_cell_measurement_reflns_used    2643
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.5330
_cell_measurement_theta_min      5.9610
_cell_volume                     2213.38(8)
_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 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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     10.00  99.00   1.00    1.00    --   36.95  19.00   0.00   89
  2  \w     20.00  66.00   1.00    1.00    --   36.95 -19.00 150.00   46
  3  \w     39.00  79.00   1.00    1.00    --   36.95-125.00 -60.00   40
  4  \w    -28.00   8.00   1.00    1.00    --   36.95 -19.00 150.00   36
  5  \w     53.00  85.00   1.00    1.99    --  111.00-111.00-150.00   32
  6  \w     42.00  94.00   1.00    1.99    --  111.00 -92.00 -60.00   52
  7  \w    108.00 148.00   1.00    1.99    --  111.00 111.00 120.00   40
  8  \w     44.00 127.00   1.00    1.99    --  111.00 -50.00 -30.00   83
  9  \w     49.00 108.00   1.00    1.99    --  111.00-111.00 120.00   59
;
_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      -0.0678303000
_diffrn_orient_matrix_UB_12      -0.0200924000
_diffrn_orient_matrix_UB_13      -0.0495223000
_diffrn_orient_matrix_UB_21      0.0135795000
_diffrn_orient_matrix_UB_22      -0.1886790000
_diffrn_orient_matrix_UB_23      -0.0149736000
_diffrn_orient_matrix_UB_31      -0.0315976000
_diffrn_orient_matrix_UB_32      -0.0383490000
_diffrn_orient_matrix_UB_33      0.0995629000
_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  0.0277
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4431
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.075
_diffrn_reflns_theta_min         4.364
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.003
_exptl_absorpt_correction_T_max  0.808
_exptl_absorpt_correction_T_min  0.256
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.888
_exptl_crystal_description       plate
_exptl_crystal_F_000             1208
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3, n-hexane'
_exptl_crystal_size_max          0.178
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_refine_diff_density_max         2.494
_refine_diff_density_min         -2.230
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2185
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0569
_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^)+(0.0278P)^2^+24.2584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1276
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2051
_reflns_number_total             2185
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01558g2.cif
_cod_data_source_block           lb071(1)_faces_manualred_new
_cod_database_code               7710826
_publcif_datablock.id            {441cde21-1cfc-4318-bb2a-dd5f1b6ad747}
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         WC18H22B1N6O2Br
_chemical_oxdiff_usercomment     'Ch/n Hex vap diff over months,'
_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. Rigid bond restraints
 C1
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C2, O2
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C2, Br2
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C1, Br1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C2 \\sim O2: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
C1: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04 within
1.7A
C2 \\sim Br2: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
C1 \\sim Br1: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
Uanis(C11) = Uanis(C12)
Uanis(C15) = Uanis(C14)
4. Others
 Fixed Sof: H11A(0.5) H11B(0.5) H11C(0.5) H15A(0.5) H15B(0.5) H15C(0.5)
 O2(0.65) Br1(0.15) Br2(0.35) O1(0.35)
5.a Ternary CH refined with riding coordinates:
 B1(H1)
5.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C23(H23)
5.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C25(H25A,H25B,
 H25C)
;
_ins_header
;
TITL LB071(1)_faces_manualred_NEW in Pna2(1) 
REM Pna2(1) (#33, found as Pc2(1)n in cab setting)
CELL 1.54184  20.262639   7.956648  13.728848  90.0000  90.0000  90.0000
ZERR    4.00   0.000333   0.000162   0.000253   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 O Br W
UNIT 72.00 88.00 4.00 24.00 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 1.341
_oxdiff_exptl_absorpt_empirical_full_min 0.857
_publcif_funding_html
;
;