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_7710824
_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 Mo N6 O2, C3 H7'
_chemical_formula_sum            'C21 H29 B Br Mo N6 O2'
_chemical_formula_weight         584.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-09
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_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            16
_cell_length_a                   38.1509(8)
_cell_length_b                   33.3659(8)
_cell_length_c                   7.97630(10)
_cell_measurement_reflns_used    16102
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.0790
_cell_measurement_theta_min      4.6060
_cell_volume                     10153.3(3)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (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     19.00 103.00   1.00    5.08    --   36.18  57.00-120.00   84
  2  \w     17.00 105.00   1.00    5.08    --   36.18  38.00 150.00   88
  3  \w     17.00 105.00   1.00    5.08    --   36.18  38.00 -30.00   88
  4  \w     27.00  90.00   1.00    5.08    --   36.18-125.00 120.00   63
  5  \w     19.00 103.00   1.00    5.08    --   36.18  57.00   0.00   84
  6  \w      3.00  30.00   1.00    5.08    --   36.18  88.00-177.26   27
  7  \w     17.00 105.00   1.00    5.08    --   36.18  38.00-120.00   88
  8  \w      3.00  30.00   1.00    5.08    --   36.18  89.00 -69.02   27
  9  \w      6.00  33.00   1.00    5.08    --   36.18  84.00-140.50   27
 10  \w     17.00 105.00   1.00    5.08    --   36.18  38.00  90.00   88
 11  \w     42.00 127.00   1.00   20.32    --  109.99 -45.00 -90.00   85
 12  \w     42.00 127.00   1.00   20.32    --  109.99 -45.00-180.00   85
 13  \w     42.00 127.00   1.00   20.32    --  109.99 -45.00  90.00   85
 14  \w     72.00 178.00   1.00   20.32    --  109.99  15.00   0.00  106
 15  \w     42.00 137.00   1.00   20.32    --  109.99 -77.00  60.00   95
 16  \w     40.00 109.00   1.00   20.32    --  109.99-111.00-120.00   69
 17  \w     40.00 109.00   1.00   20.32    --  109.99-111.00  60.00   69
 18  \w     42.00 127.00   1.00   20.32    --  109.99 -45.00   0.00   85
 19  \w     40.00 109.00   1.00   20.32    --  109.99-111.00 150.00   69
 20  \w     40.00 109.00   1.00   20.32    --  109.99-111.00 -30.00   69
 21  \w     41.00 178.00   1.00   20.32    --  109.99   0.00 -60.00  137
 22  \w      6.00  75.00   1.00    5.08    --   36.18 -99.00 -90.00   69
 23  \w      5.00  32.00   1.00    5.08    --   36.18  85.00  29.14   27
 24  \w      3.00  30.00   1.00    5.08    --   36.18  88.00  97.21   27
 25  \w    -21.00  63.00   1.00    5.08    --   36.18 -77.00 150.00   84
 26  \w    -33.00  55.00   1.00    5.08    --   36.18 -38.00-150.00   88
 27  \w    -31.00  53.00   1.00    5.08    --   36.18 -57.00 -30.00   84
 28  \w      4.00  31.00   1.00    5.08    --   36.18  87.00 149.97   27
 29  \w    -31.00  53.00   1.00    5.08    --   36.18 -57.00-180.00   84
 30  \w      7.00  42.00   1.00    5.08    --   36.18  81.00 -92.12   35
 31  \w    -31.00  53.00   1.00    5.08    --   36.18 -57.00  60.00   84
 32  \w     89.00 150.00   1.00   20.32    --  109.99  30.00  30.00   61
 33  \w     89.00 178.00   1.00   20.32    --  109.99  30.00-180.00   89
 34  \w     89.00 178.00   1.00   20.32    --  109.99  30.00  60.00   89
 35  \w     72.00 178.00   1.00   20.32    --  109.99  15.00 150.00  106
;
_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      0.0065166000
_diffrn_orient_matrix_UB_12      0.0328489000
_diffrn_orient_matrix_UB_13      -0.1323303000
_diffrn_orient_matrix_UB_21      0.0111900500
_diffrn_orient_matrix_UB_22      0.0291745500
_diffrn_orient_matrix_UB_23      0.1395260000
_diffrn_orient_matrix_UB_31      0.0382372500
_diffrn_orient_matrix_UB_32      -0.0142359500
_diffrn_orient_matrix_UB_33      -0.0183755000
_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  0.0663
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            26655
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.240
_diffrn_reflns_theta_min         4.636
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.302
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       plate
_exptl_crystal_F_000             4720
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3, n-hexane'
_exptl_crystal_size_max          0.454
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.049
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Flack x determined using 1988 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.012(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4659
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0455P)^2^+128.5334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1111
_reflns_Friedel_coverage         0.856
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4561
_reflns_number_total             4659
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01558g2.cif
_cod_data_source_block           lb063_monoi_force_2
_cod_database_code               7710824
_publcif_datablock.id            {9d16429c-b14a-4465-a564-d21e689fbff7}
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Mo Br N6 O2 B1 H21 C18'
_chemical_oxdiff_usercomment     CH/Hex
_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. Restrained distances
 C19-C20 = C20-C21
 1.52 with sigma of 0.02
 C19-C21
 2.53 with sigma of 0.04
 C19-C20 \\sim C20-C21
 with sigma of 0.02
3. Rigid bond restraints
 C1, O2B
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C1, Br1A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C3, O2A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C3, Br1B
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C14, C15
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C3 \\sim O2A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02 within 1.7A
C1 \\sim O2B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02 within 1.7A
C3 \\sim Br1B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02 within 1.7A
C1 \\sim Br1A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02 within 1.7A
C14 \\sim C15: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
C19 \\sim C20 \\sim C21: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(O2B) = Uanis(C1)
5. Rigid body (RIGU) restrains
 C19, C20, C21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: Br1A(0.75) O2A(0.75) Br1B(0.25) O2B(0.25)
7.a Ternary CH refined with riding coordinates:
 B1(H1)
7.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B)
7.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C11(H11), C16(H16)
7.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), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              18243
_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 1.679
_oxdiff_exptl_absorpt_empirical_full_min 0.613
_publcif_funding_html
;
;