Oxidation-induced coupling reactions of bi(metallacycloprop-1-ene) complexes.
Tsang, Long Yiu; Kong, Lam Cheung; Sung, Herman H. Y.; Williams, Ian D.; Jia, Guochen; Chemical communications (Cambridge, England) 60 (2024) 10946–10949; doi:10.1039/d4cc04079a

data_7133661
_publ_section_title
;
 Oxidation-induced coupling reactions of bi(metallacycloprop-1-ene)
 complexes.
;
_journal_issue                   78
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10946
_journal_page_last               10949
_journal_paper_doi               10.1039/d4cc04079a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C52 H42 Br4 P2 Re, 2(C H Cl3)'
_chemical_formula_sum            'C54 H44 Br4 Cl6 P2 Re'
_chemical_formula_weight         1473.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-08
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.11.24 svn.r209d9fb2 for OlexSys, GUI svn.r6869)
;
_audit_update_record
;
2024-02-17 deposited with the CCDC.	2024-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.0850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.08870(10)
_cell_length_b                   24.3009(2)
_cell_length_c                   19.85410(10)
_cell_measurement_reflns_used    11168
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      74.3530
_cell_measurement_theta_min      2.2870
_cell_volume                     5703.21(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.975
_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    -67.00  34.00   1.00    3.00    --  -39.95  57.00  60.00  101
  2  \w   -116.00 -18.00   1.00    3.00    --  -39.95 -37.00 -90.00   98
  3  \w    -21.00  74.00   1.00    3.00    --   39.95 -77.00-180.00   95
  4  \w     77.00 168.00   1.00    8.00    --  107.44  61.00-180.00   91
  5  \w     29.00 109.00   1.00    8.00    --  107.44-111.00-180.00   80
  6  \w     23.00  51.00   1.00    8.00    --  107.44 -94.00-120.00   28
  7  \w     77.00 175.00   1.00    8.00    --  107.44  61.00 120.00   98
  8  \w     60.00 106.00   1.00    8.00    --  107.44 -94.00-120.00   46
  9  \w     83.00 175.00   1.00    8.00    --  107.44  30.00  90.00   92
 10  \w     29.00 106.00   1.00    8.00    --  107.44 -94.00 -30.00   77
 11  \w     41.00 134.00   1.00    8.00    --  107.44 -45.00 150.00   93
 12  \w     30.00 129.00   1.00    8.00    --  107.44 -77.00   0.00   99
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0647011000
_diffrn_orient_matrix_UB_12      -0.0348321000
_diffrn_orient_matrix_UB_13      -0.0439493000
_diffrn_orient_matrix_UB_21      -0.0623562000
_diffrn_orient_matrix_UB_22      -0.0519815000
_diffrn_orient_matrix_UB_23      0.0165487000
_diffrn_orient_matrix_UB_31      -0.0944228000
_diffrn_orient_matrix_UB_32      0.0104187000
_diffrn_orient_matrix_UB_33      -0.0638721000
_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  0.0350
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16796
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.256
_diffrn_reflns_theta_min         3.638
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    10.835
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_description       block
_exptl_crystal_F_000             2860
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.397
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         5672
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0467P)^2^+22.0963P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0896
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5248
_reflns_number_total             5672
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04079a2.cif
_cod_data_source_block           tsang28cu_173k_auto
_cod_depositor_comments
'Adding full bibliography for 7133660--7133663.cif.'
_cod_database_code               7133661
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 Cl2A-Cl1A
 2.88 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C1S) \\sim Ueq, Uanis(Cl3) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(Cl1)
\\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.005
Uanis(C1SA) \\sim Ueq, Uanis(Cl3A) \\sim Ueq, Uanis(Cl2A) \\sim Ueq,
Uanis(Cl1A) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.005
4. Rigid body (RIGU) restrains
 Cl1, Cl2, Cl3, C1S
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl1A, Cl2A, Cl3A, C1SA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: Cl1(0.666667) Cl2(0.666667) Cl3(0.666667) C1S(0.666667)
 H1S(0.666667) Cl1A(0.333333) Cl2A(0.333333) Cl3A(0.333333) C1SA(0.333333)
 H1SA(0.333333)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C1S(H1S), C1SA(H1SA)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C32(H32),
  C33(H33), C34(H34), C35(H35), C36(H36)
;
_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 3.035
_oxdiff_exptl_absorpt_empirical_full_min 0.674