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_7710821
_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 Cl2 N6 O2 W, C3 H6'
_chemical_formula_sum            'C21 H28 Au B Cl2 N6 O2 W'
_chemical_formula_weight         859.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-15 deposited with the CCDC.	2022-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.8070(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3472(2)
_cell_length_b                   10.47460(10)
_cell_length_c                   19.2527(3)
_cell_measurement_reflns_used    5031
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.5190
_cell_measurement_theta_min      4.8180
_cell_volume                     2624.69(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_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 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_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     -5.00  66.00   1.00    1.75    --   37.05 -19.00 120.00   71
  2  \w     11.00  75.00   1.00    1.75    --   37.05 -99.00   0.00   64
  3  \w    -33.00  -6.00   1.00    1.75    --   37.05 -19.00 120.00   27
  4  \w    -18.00  64.00   1.00    1.75    --   37.05 -77.00  60.00   82
  5  \w      6.00  75.00   1.00    1.75    --   37.05 -99.00 150.00   69
  6  \w     51.00 122.00   1.00    7.10    --  111.00 -50.00-120.00   71
  7  \w     43.00 124.00   1.00    7.10    --  111.00 -38.00 -60.00   81
  8  \w    150.00 178.00   1.00    7.10    --  111.00  50.00-180.00   28
  9  \w     95.00 120.00   1.00    7.10    --  111.00  50.00-180.00   25
 10  \w     44.00 128.00   1.00    7.10    --  111.00 -50.00  30.00   84
 11  \w     41.00  99.00   1.00    7.10    --  111.00-111.00   0.00   58
 12  \w     51.00 105.00   1.00    7.10    --  111.00 -92.00  30.00   54
 13  \w     66.00 175.00   1.00    7.10    --  111.00  12.00   0.00  109
;
_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      -0.0839014000
_diffrn_orient_matrix_UB_12      0.0305722000
_diffrn_orient_matrix_UB_13      -0.0668767000
_diffrn_orient_matrix_UB_21      -0.0816782000
_diffrn_orient_matrix_UB_22      -0.0593668000
_diffrn_orient_matrix_UB_23      0.0354226000
_diffrn_orient_matrix_UB_31      -0.0173287000
_diffrn_orient_matrix_UB_32      0.1310427000
_diffrn_orient_matrix_UB_33      0.0317910000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9761
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.099
_diffrn_reflns_theta_min         4.543
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.463
_exptl_absorpt_correction_T_max  0.637
_exptl_absorpt_correction_T_min  0.145
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (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 orange'
_exptl_crystal_density_diffrn    2.174
_exptl_crystal_description       plate
_exptl_crystal_F_000             1616
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF, cyclohexane'
_exptl_crystal_size_max          0.148
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.041
_refine_diff_density_max         1.132
_refine_diff_density_min         -1.341
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         5126
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0413P)^2^+2.5566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0866
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4570
_reflns_number_total             5126
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01558g2.cif
_cod_data_source_block           lb049_faces
_cod_database_code               7710821
_publcif_datablock.id            {f9be8dc0-c2e0-47c2-aa81-cb07c8c3c1c3}
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C21H28BN6O2Cl2WAu
_chemical_oxdiff_usercomment     'THF/Cyclohex vap diff @ 5 degC'
_reflns_odcompleteness_completeness 99.07
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C3) = Uanis(C2)
Uanis(O2) = Uanis(O1)
3.a Ternary CH refined with riding coordinates:
 B1(H1)
3.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B)
3.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C11(H11), C16(H16)
3.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C18(H18A,H18B,H18C)
;
_ins_header
;
TITL LB049_faces in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  13.347158  10.474604  19.252674  90.0000 102.8070  90.0000
ZERR    4.00   0.000178   0.000143   0.000277   0.0000   0.0014   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H B N O Cl W Au
UNIT 84.00 112.00 4.00 24.00 8.00 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 1.284
_oxdiff_exptl_absorpt_empirical_full_min 0.795
_publcif_funding_html
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;