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_7133662
_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         'C64 H50 Cl4 P2 Re, 2[CH2Cl2]'
_chemical_formula_sum            'C64 H50 Cl4 P2 Re'
_chemical_formula_weight         1208.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 107.9434(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5823(3)
_cell_length_b                   22.9599(3)
_cell_length_c                   18.0278(3)
_cell_measurement_reflns_used    11366
_cell_measurement_temperature    173
_cell_measurement_theta_max      75.7200
_cell_measurement_theta_min      3.1820
_cell_volume                     6136.06(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.69a (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      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1788
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_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     85.00 176.00   1.00   16.00    --  113.00  45.00  30.00   91
  2  \w    -80.00 -10.00   1.00    5.00    --  -39.95 125.00 -90.00   70
  3  \w   -116.00  -3.00   1.00    5.00    --  -39.95 -19.00-180.00  113
  4  \w   -115.00 -38.00   1.00    5.00    --  -39.95 -37.00 120.00   77
  5  \w     35.00  78.00   1.00    5.00    --   39.95-125.00 -90.00   43
  6  \w      6.00  80.00   1.00    5.00    --   39.95 -99.00  90.00   74
  7  \w     82.00 172.00   1.00   16.00    --  113.00  30.00  90.00   90
  8  \w    104.00 178.00   1.00   16.00    --  113.00 111.00 -90.00   74
  9  \w    103.00 177.00   1.00   16.00    --  113.00  77.00 -30.00   74
 10  \w     35.00 109.00   1.00   16.00    --  113.00-111.00-150.00   74
 11  \w     35.00 109.00   1.00   16.00    --  113.00-111.00 120.00   74
 12  \w     29.00 107.00   1.00   16.00    --  113.00 -94.00-120.00   78
 13  \w     35.00 142.00   1.00   16.00    --  113.00 -30.00-150.00  107
 14  \w     43.00 146.00   1.00   16.00    --  113.00 -77.00 -60.00  103
;
_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      -0.0372332000
_diffrn_orient_matrix_UB_12      -0.0555933000
_diffrn_orient_matrix_UB_13      0.0266806000
_diffrn_orient_matrix_UB_21      0.0753949000
_diffrn_orient_matrix_UB_22      -0.0361003000
_diffrn_orient_matrix_UB_23      -0.0165421000
_diffrn_orient_matrix_UB_31      0.0607483000
_diffrn_orient_matrix_UB_32      0.0105645000
_diffrn_orient_matrix_UB_33      0.0843175000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39181
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.786
_diffrn_reflns_theta_min         3.216
_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    6.239
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       plate
_exptl_crystal_F_000             2428
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.471
_refine_diff_density_min         -1.281
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         12655
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0583P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1167
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9272
_reflns_number_total             12655
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04079a2.cif
_cod_data_source_block           tsang6cu_173k
_cod_depositor_comments
'Adding full bibliography for 7133660--7133663.cif.'
_cod_original_cell_volume        6136.07(18)
_cod_database_code               7133662
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.746
_shelx_estimated_absorpt_t_min   0.521
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C4(H4)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16),
 C17(H17), C22(H22), C23(H23), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30),
  C31(H31), C32(H32), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
 C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C62(H62), C63(H63), C64(H64),
  C65(H65), C66(H66), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76),
 C82(H82), C83(H83), C84(H84), C85(H85), C86(H86), C92(H92), C93(H93), C94(H94),
  C95(H95), C96(H96)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 374 electrons were 
found in a volume of 1400\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[CH2Cl2] per Asymmetric Unit 
which account for 336 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 1.331
_oxdiff_exptl_absorpt_empirical_full_min 0.429