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_1568013
_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         'C52 H42 Cl3 P2 Re, 2(C H2 Cl2)'
_chemical_formula_sum            'C54 H46 Cl7 P2 Re'
_chemical_formula_weight         1191.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-09-07 deposited with the CCDC.	2022-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                85.943(4)
_cell_angle_beta                 80.643(4)
_cell_angle_gamma                72.033(4)
_cell_formula_units_Z            2
_cell_length_a                   10.9390(6)
_cell_length_b                   13.1090(6)
_cell_length_c                   18.4122(10)
_cell_measurement_reflns_used    10222
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      76.7060
_cell_measurement_theta_min      2.4250
_cell_volume                     2477.5(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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1788
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.953
_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     91.00 174.00   1.00    6.00    --  113.00  45.00 -30.00   83
  2  \w    -79.00  -6.00   1.00    3.00    --  -39.95 125.00  90.00   73
  3  \w   -116.00 -18.00   1.00    3.00    --  -39.95 -37.00-180.00   98
  4  \w   -115.00 -14.00   1.00    3.00    --  -39.95 -37.00 -90.00  101
  5  \w     31.00  93.00   1.00    3.00    --   39.95-125.00   0.00   62
  6  \w    -14.00  43.00   1.00    3.00    --   39.95 -77.00  60.00   57
  7  \w     37.00 138.00   1.00    6.00    --  113.00 -72.00 161.00  101
  8  \w    104.00 178.00   1.00    6.00    --  113.00 111.00 -90.00   74
  9  \w    107.00 176.00   1.00    6.00    --  113.00  77.00-120.00   69
 10  \w    116.00 143.00   1.00    6.00    --  113.00 -30.00 150.00   27
 11  \w     76.00 109.00   1.00    6.00    --  113.00-111.00 -60.00   33
 12  \w     37.00 103.00   1.00    6.00    --  113.00 -30.00 150.00   66
 13  \w     35.00 109.00   1.00    6.00    --  113.00-111.00 120.00   74
 14  \w     55.00 144.00   1.00    6.00    --  113.00 -30.00 -90.00   89
 15  \w     34.00 141.00   1.00    6.00    --  113.00 -77.00 -60.00  107
;
_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      -0.0106960000
_diffrn_orient_matrix_UB_12      -0.0995552000
_diffrn_orient_matrix_UB_13      0.0472114000
_diffrn_orient_matrix_UB_21      0.0920112000
_diffrn_orient_matrix_UB_22      0.0183442000
_diffrn_orient_matrix_UB_23      0.0493349000
_diffrn_orient_matrix_UB_31      -0.1175921000
_diffrn_orient_matrix_UB_32      0.0708893000
_diffrn_orient_matrix_UB_33      0.0503164000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16048
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.189
_diffrn_reflns_theta_min         2.433
_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    9.164
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79297
_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    1.597
_exptl_crystal_description       block
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.703
_refine_diff_density_min         -1.093
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         10015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0283
_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^)+(0.0313P)^2^+0.9803P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0699
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9113
_reflns_number_total             10015
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc05378k2.cif
_cod_data_source_block           tsang4a_173k
_cod_depositor_comments
'Adding full bibliography for 1568013--1568015.cif.'
_cod_database_code               1568013
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Re P3 Cl2 C40 H38 O2 '
_shelx_estimated_absorpt_t_max   0.657
_shelx_estimated_absorpt_t_min   0.528
_reflns_odcompleteness_completeness 98.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C1(H1), C3(H3)
1.b Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB)
1.c 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), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36),
  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)
;
_shelx_res_checksum              8338
_shelx_hkl_checksum              58186
_olex2_date_sample_data_collection 2021-05-01
_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 1.201
_oxdiff_exptl_absorpt_empirical_full_min 0.799