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_7133663
_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         'C76 H56 Cl4 N2 P2 Re, 7[CH2Cl2]'
_chemical_formula_sum            'C83 H70 Cl18 N2 P2 Re'
_chemical_formula_weight         1981.65
_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             2024-02-23
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-02-26 deposited with the CCDC.	2024-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.713(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.6823(7)
_cell_length_b                   18.6829(7)
_cell_length_c                   24.3283(8)
_cell_measurement_reflns_used    11121
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.2970
_cell_measurement_theta_min      3.0160
_cell_volume                     8367.8(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1788
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.978
_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     45.00 109.00   1.00   38.00    --  113.00-111.00-120.00   64
  2  \w    -73.00 -10.00   1.00   12.00    --  -40.20 125.00 -30.00   63
  3  \w    -89.00  -6.00   1.00   12.00    --  -40.20 -19.00-120.00   83
  4  \w   -116.00 -17.00   1.00   12.00    --  -40.20 -37.00-180.00   99
  5  \w    -14.00  73.00   1.00   12.00    --   40.20 -77.00  90.00   87
  6  \w     42.00  86.00   1.00   12.00    --   40.20-125.00 -60.00   44
  7  \w     29.00 105.00   1.00   38.00    --  113.00 -94.00 -30.00   76
  8  \w     49.00 144.00   1.00   38.00    --  113.00 -30.00 -90.00   95
  9  \w     82.00 118.00   1.00   38.00    --  113.00  30.00 150.00   36
 10  \w     50.00 109.00   1.00   38.00    --  113.00-111.00  60.00   59
 11  \w    121.00 178.00   1.00   38.00    --  113.00  30.00 150.00   57
 12  \w    108.00 178.00   1.00   38.00    --  113.00 111.00  30.00   70
 13  \w     89.00 171.00   1.00   38.00    --  113.00  45.00  90.00   82
 14  \w     38.00 144.00   1.00   38.00    --  113.00 -30.00  90.00  106
 15  \w     35.00 140.00   1.00   38.00    --  113.00 -77.00  60.00  105
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0381873000
_diffrn_orient_matrix_UB_12      0.0351295000
_diffrn_orient_matrix_UB_13      0.0604467000
_diffrn_orient_matrix_UB_21      -0.0727975000
_diffrn_orient_matrix_UB_22      0.0333360000
_diffrn_orient_matrix_UB_23      -0.0025224000
_diffrn_orient_matrix_UB_31      -0.0158886000
_diffrn_orient_matrix_UB_32      -0.0666672000
_diffrn_orient_matrix_UB_33      0.0304011000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1086
_diffrn_reflns_av_unetI/netI     0.1273
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            52122
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.944
_diffrn_reflns_theta_min         2.400
_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    8.850
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       block
_exptl_crystal_F_000             3972
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.192
_refine_diff_density_min         -1.716
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         17288
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0733
_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^)+(0.0893P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1818
_refine_ls_wR_factor_ref         0.2027
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10965
_reflns_number_total             17288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04079a2.cif
_cod_data_source_block           tsang7a_100k
_cod_depositor_comments
'Adding full bibliography for 7133660--7133663.cif.'
_cod_original_cell_volume        8367.8(5)
_cod_database_code               7133663
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Re Cl4 P C40 H38'
_shelx_estimated_absorpt_t_max   0.619
_shelx_estimated_absorpt_t_min   0.538
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid body (RIGU) restrains
 Re1, P1, P2, C1, C2, C3, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Ternary CH refined with riding coordinates:
 C1(H1), C4(H4)
3.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20),
 C21(H21), C24(H24), C25(H25), C26(H26), C27(H27), C32(H32), C33(H33), C35(H35),
  C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C44(H44), C45(H45),
 C46(H46), C47(H47), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C58(H58),
  C59(H59), C60(H60), C61(H61), C62(H62), C64(H64), C65(H65), C66(H66),
 C67(H67), C68(H68), C70(H70), C71(H71), C72(H72), C73(H73), C74(H74), C76(H76),
  C77(H77), C78(H78), C79(H79), C80(H80), C82(H82), C83(H83), C84(H84),
 C85(H85), C86(H86)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1195 electrons were 
found in a volume of 3116\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
7[CH2Cl2] per Asymmetric Unit 
which account for 1176 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.493
_oxdiff_exptl_absorpt_empirical_full_min 0.697