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_7133660
_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 Cl4 P2 Re, 2(H2 C Cl2)'
_chemical_formula_sum            'C54 H46 Cl8 P2 Re'
_chemical_formula_weight         1226.65
_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
_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                 102.929(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0537(3)
_cell_length_b                   23.1354(5)
_cell_length_c                   20.0755(3)
_cell_measurement_reflns_used    5547
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      75.8860
_cell_measurement_theta_min      4.2240
_cell_volume                     5456.5(2)
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      172.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1788
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.959
_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     39.00 143.00   1.00    8.00    --  113.00 -61.00  30.00  104
  2  \w   -114.00 -10.00   1.00    3.00    --  -39.95 -57.00 -30.00  104
  3  \w     27.00  97.00   1.00    3.00    --   39.95-125.00 -30.00   70
  4  \w     28.00  93.00   1.00    3.00    --   39.95-125.00-180.00   65
  5  \w     36.00 136.00   1.00    8.00    --  113.00 -30.00-150.00  100
  6  \w    103.00 178.00   1.00    8.00    --  113.00  77.00 150.00   75
  7  \w     46.00 167.00   1.00    8.00    --  113.00 -15.00 -30.00  121
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Mo at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0422815000
_diffrn_orient_matrix_UB_12      0.0087462000
_diffrn_orient_matrix_UB_13      0.0662649000
_diffrn_orient_matrix_UB_21      0.0541856000
_diffrn_orient_matrix_UB_22      -0.0580168000
_diffrn_orient_matrix_UB_23      0.0275442000
_diffrn_orient_matrix_UB_31      0.1116631000
_diffrn_orient_matrix_UB_32      0.0314627000
_diffrn_orient_matrix_UB_33      0.0324831000
_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  0.0281
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9902
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.768
_diffrn_reflns_theta_min         4.221
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Mo
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    8.780
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70939
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       block
_exptl_crystal_F_000             2444
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.807
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         5536
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0434P)^2^+13.1601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0840
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5088
_reflns_number_total             5536
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04079a2.cif
_cod_data_source_block           tsang5cu_173k
_cod_depositor_comments
'Adding full bibliography for 7133660--7133663.cif.'
_cod_database_code               7133660
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.668
_shelx_estimated_absorpt_t_min   0.474
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 Cl1S-Cl2A
 2.75 with sigma of 0.02
 Cl3S-Cl4S
 2.75 with sigma of 0.02
 Cl1S-Cl2S
 2.75 with sigma of 0.02
 Cl3S-C2S \\sim Cl4S-C2S
 with sigma of 0.02
 Cl1S-C1S \\sim Cl2S-C1S \\sim Cl2A-C1S
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C2S) \\sim Ueq, Uanis(Cl3S) \\sim Ueq, Uanis(Cl4S) \\sim Ueq: with sigma
of 0.002 and sigma for terminal atoms of 0.003
Uanis(C1S) \\sim Ueq, Uanis(Cl2S) \\sim Ueq, Uanis(Cl2A) \\sim Ueq, Uanis(Cl1S)
\\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.003
4. Rigid body (RIGU) restrains
 Cl3S, Cl4S, C2S
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl1S, Cl2A, Cl2S, C1S
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: Cl1S(0.9) Cl2A(0.1) Cl2S(0.8) Cl3S(0.1) Cl4S(0.1) C1S(0.9) C2S(0.1)
6.a Ternary CH refined with riding coordinates:
 C1(H1)
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 1.384
_oxdiff_exptl_absorpt_empirical_full_min 0.826