Synthesis and characterization of bi(metallacycloprop-1-ene) complexes.
Bai, Wei; Tsang, Long Yiu; Wang, Yilun; Li, Yang; Sung, Herman H. Y.; Williams, Ian D.; Jia, Guochen; Chemical science 14 (2022) 96–102; doi:10.1039/d2sc05378k

data_1568014
_publ_section_title
;
 Synthesis and characterization of bi(metallacycloprop-1-ene) complexes.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              96
_journal_page_last               102
_journal_paper_doi               10.1039/d2sc05378k
_journal_volume                  14
_journal_year                    2022
_chemical_formula_moiety         'C32 H36 Cl3 P2 Re'
_chemical_formula_sum            'C32 H36 Cl3 P2 Re'
_chemical_formula_weight         775.10
_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     direct
_audit_creation_date             2022-06-08
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-09-07 deposited with the CCDC.	2022-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.276(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0820(2)
_cell_length_b                   18.4374(3)
_cell_length_c                   15.6667(3)
_cell_measurement_reflns_used    5491
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      74.2600
_cell_measurement_theta_min      4.8000
_cell_volume                     3056.66(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_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     35.00  62.00   1.00    5.00    --  110.57-111.00  30.00   27
  2  \w    -67.00  36.00   1.00    2.00    --  -40.57  77.00  30.00  103
  3  \w    -69.00  36.00   1.00    2.00    --  -40.57  77.00 150.00  105
  4  \w    -70.00  33.00   1.00    2.00    --  -40.57  57.00 -60.00  103
  5  \w     84.00 111.00   1.00    5.00    --  110.57-111.00  30.00   27
  6  \w     38.00 107.00   1.00    5.00    --  110.57 -94.00  90.00   69
  7  \w     42.00 141.00   1.00    5.00    --  110.57 -30.00   0.00   99
  8  \w     80.00 167.00   1.00    5.00    --  110.57  30.00   0.00   87
  9  \w    100.00 154.00   1.00    5.00    --  110.57 111.00  60.00   54
 10  \w     96.00 177.00   1.00    5.00    --  110.57  61.00  30.00   81
 11  \w     34.00 113.00   1.00    5.00    --  110.57-111.00-120.00   79
 12  \w     38.00 139.00   1.00    5.00    --  110.57 -77.00 -90.00  101
 13  \w     26.00  88.00   1.00    5.00    --  110.57 -94.00-180.00   62
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8945
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.541
_diffrn_reflns_theta_min         4.797
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    11.330
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.684
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.079
_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     175
_refine_ls_number_reflns         3107
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0174
_refine_ls_R_factor_gt           0.0167
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0222P)^2^+2.9616P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0417
_refine_ls_wR_factor_ref         0.0421
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3016
_reflns_number_total             3107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc05378k2.cif
_cod_data_source_block           bai80cult
_cod_depositor_comments
'Adding full bibliography for 1568013--1568015.cif.'
_cod_database_code               1568014
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26)
2.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              97643
_shelx_hkl_checksum              98725
_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
;