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_7710823
_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         'C18 H22 Au B Cl2 Mo N6 O2'
_chemical_formula_sum            'C18 H22 Au B Cl2 Mo N6 O2'
_chemical_formula_weight         729.03
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-28
_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                 108.0220(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.4253(3)
_cell_length_b                   10.96890(10)
_cell_length_c                   19.7589(2)
_cell_measurement_reflns_used    10072
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.9260
_cell_measurement_theta_min      4.4170
_cell_volume                     5240.15(10)
_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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 32.5190
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.995
_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     24.00 103.00   1.00    2.00    --   36.95  57.00 150.00   79
  2  \w     35.00  89.00   1.00    2.00    --   36.95-125.00  90.00   54
  3  \w    -27.00  56.00   1.00    2.00    --   36.95 -38.00-120.00   83
  4  \w    -29.00  48.00   1.00    2.00    --   36.95 -57.00  30.00   77
  5  \w     95.00 173.00   1.00    8.00    --  111.00  38.00 -90.00   78
  6  \w     47.00 127.00   1.00    8.00    --  111.00 -50.00 120.00   80
  7  \w     66.00 135.00   1.00    8.00    --  111.00 -25.00  90.00   69
  8  \w     45.00 107.00   1.00    8.00    --  111.00-125.00  11.00   62
  9  \w     41.00 109.00   1.00    8.00    --  111.00-111.00  60.00   68
 10  \w    103.00 174.00   1.00    8.00    --  111.00  77.00 120.00   71
 11  \w     42.00 109.00   1.00    8.00    --  111.00-111.00  30.00   67
 12  \w     83.00 109.00   1.00    8.00    --  111.00-111.00 120.00   26
 13  \w     50.00 129.00   1.00    8.00    --  111.00 -64.00  30.00   79
;
_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      0.0469035000
_diffrn_orient_matrix_UB_12      0.0900459000
_diffrn_orient_matrix_UB_13      0.0020384000
_diffrn_orient_matrix_UB_21      -0.0373535000
_diffrn_orient_matrix_UB_22      0.1072704000
_diffrn_orient_matrix_UB_23      0.0062551000
_diffrn_orient_matrix_UB_31      0.0214911000
_diffrn_orient_matrix_UB_32      -0.0105959000
_diffrn_orient_matrix_UB_33      0.0817862000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21904
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.127
_diffrn_reflns_theta_min         3.656
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.381
_exptl_absorpt_correction_T_max  0.531
_exptl_absorpt_correction_T_min  0.140
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_description       plate
_exptl_crystal_F_000             2784
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3, n-hexane'
_exptl_crystal_size_max          0.163
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.049
_refine_diff_density_max         2.288
_refine_diff_density_min         -1.131
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         10256
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0233P)^2^+65.0124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1021
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9646
_reflns_number_total             10256
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01558g2.cif
_cod_data_source_block           lb048_faces
_cod_depositor_comments
;

2024-09-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C36 H44 Au2 B2 Cl4 Mo2 N12 O4'
_cod_original_formula_weight         1458.06
_cod_original_formula_moiety         '2(C18 H22 Au B Cl2 Mo N6 O2)'
_cod_original_formula_units_Z            4
_cod_database_code               7710823
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C19H22O2N6Cl5B1Mo1Au1
_chemical_oxdiff_usercomment     'Vap diff, CHCl3/nhex @ 5 degC'
_reflns_odcompleteness_completeness 99.15
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C8B) = Uanis(C7B)
3.a Ternary CH refined with riding coordinates:
 B1A(H1A), B1B(H1B)
3.b Aromatic/amide H refined with riding coordinates:
 C6A(H6A), C11A(H11A), C16A(H16A), C6B(H6B), C11B(H11B), C16B(H16B)
3.c Idealised Me refined as rotating group:
 C4A(H4AA,H4AB,H4AC), C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C13A(H13A,H13B,
 H13C), C14A(H14A,H14B,H14C), C18A(H18A,H18B,H18C), C4B(H4BA,H4BB,H4BC),
 C8B(H8BA,H8BB,H8BC), C9B(H9BA,H9BB,H9BC), C13B(H13D,H13E,H13F), C14B(H14D,H14E,
 H14F), C18B(H18D,H18E,H18F)
;
_ins_header
;
TITL LB048_faces in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 1.54184  25.425288  10.968927  19.758860  90.0000 108.0216  90.0000
ZERR    8.00   0.000296   0.000105   0.000191   0.0000   0.0012   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H B N O Cl Mo Au
UNIT 152.00 176.00 8.00 48.00 16.00 40.00 8.00 8.00
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 1.333
_oxdiff_exptl_absorpt_empirical_full_min 0.834