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_7710830
_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 Au B Br Cl Mo N6 O2, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C18.5 H23 Au B Br Cl2 Mo N6 O2'
_chemical_formula_weight         815.95
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-29
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.04.28 svn.r794ee209 for OlexSys, GUI svn.r6317)
;
_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            8
_cell_length_a                   19.91210(10)
_cell_length_b                   10.88540(10)
_cell_length_c                   23.86150(10)
_cell_measurement_reflns_used    31611
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.6910
_cell_measurement_theta_min      4.0450
_cell_volume                     5172.01(6)
_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      150.00(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 1.000
_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    -63.00 -12.00   1.00    1.00    --  -36.95 -19.00-150.00   51
  2  \w    -39.00   0.00   1.00    1.00    --  -36.95  38.00  90.00   39
  3  \w   -101.00 -66.00   1.00    1.00    --  -36.95 -19.00-150.00   35
  4  \w     37.00  88.00   1.00    1.00    --   36.95-125.00 -30.00   51
  5  \w    -17.00  11.00   1.00    1.00    --   36.95 -38.00  90.00   28
  6  \w     21.00  86.00   1.00    1.00    --   36.95-117.00 142.00   65
  7  \w    -32.00 100.00   1.00    1.00    --   36.95   0.00  30.00  132
  8  \w    -18.00  64.00   1.00    1.00    --   36.95 -77.00   0.00   82
  9  \w    -27.00  52.00   1.00    1.00    --   36.95 -57.00-180.00   79
 10  \w     18.00  53.00   1.00    1.00    --   36.95 -38.00  90.00   35
 11  \w     43.00 116.00   1.00    1.00    --  111.00 -50.00  60.00   73
 12  \w     68.00 109.00   1.00    1.00    --  111.00-111.00-150.00   41
 13  \w     43.00 138.00   1.00    1.00    --  111.00 -77.00-180.00   95
 14  \w     41.00 109.00   1.00    1.00    --  111.00-111.00   0.00   68
 15  \w     46.00 126.00   1.00    1.00    --  111.00 -38.00-120.00   80
 16  \w     60.00 100.00   1.00    1.00    --  111.00 -92.00 120.00   40
 17  \w     60.00 109.00   1.00    1.00    --  111.00-111.00  90.00   49
 18  \w     97.00 177.00   1.00    1.00    --  111.00  38.00  30.00   80
 19  \w     86.00 177.00   1.00    1.00    --  111.00  25.00  90.00   91
 20  \w     85.00 120.00   1.00    1.00    --  111.00 -25.00 150.00   35
 21  \w     84.00 109.00   1.00    1.00    --  111.00-111.00 -60.00   25
 22  \w     47.00  73.00   1.00    1.00    --  111.00-111.00 -60.00   26
 23  \w    119.00 177.00   1.00    1.00    --  111.00 111.00 150.00   58
 24  \w    103.00 178.00   1.00    1.00    --  111.00  77.00-180.00   75
 25  \w     42.00  83.00   1.00    1.00    --  111.00 -25.00 150.00   41
 26  \w    121.00 177.00   1.00    1.00    --  111.00  77.00-150.00   56
 27  \w     41.00 130.00   1.00    1.00    --  111.00 -25.00  60.00   89
;
_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      -0.0141779000
_diffrn_orient_matrix_UB_12      0.0007330000
_diffrn_orient_matrix_UB_13      0.0634548000
_diffrn_orient_matrix_UB_21      0.0429543000
_diffrn_orient_matrix_UB_22      -0.1166668000
_diffrn_orient_matrix_UB_23      0.0069577000
_diffrn_orient_matrix_UB_31      0.0627974000
_diffrn_orient_matrix_UB_32      0.0800988000
_diffrn_orient_matrix_UB_33      0.0095495000
_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  0.0314
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            37610
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.125
_diffrn_reflns_theta_min         3.705
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.429
_exptl_absorpt_correction_T_max  0.336
_exptl_absorpt_correction_T_min  0.034
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.79a (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    2.096
_exptl_crystal_description       block
_exptl_crystal_F_000             3096
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.367
_exptl_crystal_size_mid          0.245
_exptl_crystal_size_min          0.085
_refine_diff_density_max         1.383
_refine_diff_density_min         -1.774
_refine_diff_density_rms         0.158
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.258(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         10173
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0617P)^2^+6.6018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0802
_reflns_Friedel_coverage         0.945
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                10151
_reflns_number_total             10173
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01558g2.cif
_cod_data_source_block           lb051(2)_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            'C37 H46 Au2 B2 Br2 Cl4 Mo2 N12 O4'
_cod_original_formula_weight         1631.91
_cod_original_formula_moiety         '2(C18 H22 Au B Br Cl Mo N6 O2), C H2 Cl2'
_cod_original_formula_units_Z            4
_cod_database_code               7710830
_publcif_datablock.id            {c1aeb0f5-42f9-4c5a-8782-cd5c31d202aa}
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C37H46Au2B2Br2Cl4Mo2N12O4
_chemical_oxdiff_usercomment     'Vap diff, DCM/nHex, 5 degC o/n'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.742(8)
 0.258(8)
2. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, {H9AA,H9AB,H9AC} of C9A, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  {H8BA,H8BB,H8BC} of C8B, {H18A,H18B,H18C} of C18A, {H13A,H13B,H13C} of C13A,
   {H14A,H14B,H14C} of C14A, {H9BA,H9BB,H9BC} of C9B, {H14D,H14E,H14F} of C14B,
  {H13D,H13E,H13F} of C13B, {H8AA,H8AB,H8AC} of C8A, {H4AA,H4AB,H4AC} of C4A,
  {H18D,H18E,H18F} of C18B, {H4BA,H4BB,H4BC} of C4B
3. Rigid bond restraints
 C15B, C16B, C17B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C15B \\sim C16B \\sim C17B: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 1.7A
Uanis(C8A) = Uanis(C7A)
Uanis(C8B) = Uanis(C7B)
5.a Ternary CH refined with riding coordinates:
 B1A(H1A), B1B(H1B)
5.b Secondary CH2 refined with riding coordinates:
 C01T(H01A,H01B)
5.c Aromatic/amide H refined with riding coordinates:
 C11B(H11B), C6B(H6B), C16B(H16B), C16A(H16A), C11A(H11A), C6A(H6A)
5.d Idealised Me refined as rotating group:
 C9A(H9AA,H9AB,H9AC), C13A(H13A,H13B,H13C), C14A(H14A,H14B,H14C), C9B(H9BA,
 H9BB,H9BC), C4B(H4BA,H4BB,H4BC), C14B(H14D,H14E,H14F), C13B(H13D,H13E,H13F),
 C4A(H4AA,H4AB,H4AC), C18B(H18D,H18E,H18F), C8A(H8AA,H8AB,H8AC), C18A(H18A,H18B,
 H18C), C8B(H8BA,H8BB,H8BC)
;
_shelx_res_checksum              2738
_ins_header
;
TITL LB051(2)_faces in Pca2(1) 
REM Pca2(1) (#29, found as Pbc2(1) in ba-c setting)
CELL 1.54184  19.912119  10.885407  23.861513  90.0000  90.0000  90.0000
ZERR    4.00   0.000102   0.000052   0.000117   0.0000   0.0000   0.0000
LATT -1
SYMM -x,-y, z+1/2 
SYMM  x+1/2,-y, z 
SYMM -x+1/2, y, z+1/2 
SFAC C H B N O Cl Br Mo Au
UNIT 148.00 184.00 8.00 48.00 16.00 16.00 8.00 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 1.375
_oxdiff_exptl_absorpt_empirical_full_min 0.679
_publcif_funding_html
;
;