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_1568015
_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_absolute_configuration ad
_chemical_formula_moiety         'C42 H38 Cl3 P2 Re'
_chemical_formula_sum            'C42 H38 Cl3 P2 Re'
_chemical_formula_weight         897.21
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-03-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2022-09-07 deposited with the CCDC.	2022-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.4928(3)
_cell_length_b                   11.58031(15)
_cell_length_c                   13.76598(19)
_cell_measurement_reflns_used    4280
_cell_measurement_temperature    220.02(10)
_cell_measurement_theta_max      75.5410
_cell_measurement_theta_min      4.2440
_cell_volume                     3745.09(9)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      220.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.960
_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    -69.00  31.00   1.00    3.00    --  -40.57  57.00-120.00  100
  2  \w     70.00  96.00   1.00    3.00    --   40.57-125.00 150.00   26
  3  \w     29.00 103.00   1.00    8.00    --  110.57 -94.00   0.00   74
  4  \w     49.00 140.00   1.00    8.00    --  110.57 -30.00-180.00   91
  5  \w     85.00 178.00   1.00    8.00    --  110.57  45.00-180.00   93
;
_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      0.0565254000
_diffrn_orient_matrix_UB_12      -0.0645280000
_diffrn_orient_matrix_UB_13      -0.0161777000
_diffrn_orient_matrix_UB_21      -0.0308016000
_diffrn_orient_matrix_UB_22      -0.1163199000
_diffrn_orient_matrix_UB_23      0.0144076000
_diffrn_orient_matrix_UB_31      -0.0125308000
_diffrn_orient_matrix_UB_32      -0.0058187000
_diffrn_orient_matrix_UB_33      -0.1096878000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8207
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.619
_diffrn_reflns_theta_min         4.256
_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    9.344
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85356
_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    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.140
_refine_diff_density_min         -1.431
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.025(16)
_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     435
_refine_ls_number_reflns         4739
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0660P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.0996
_reflns_Friedel_coverage         0.215
_reflns_Friedel_fraction_full    0.245
_reflns_Friedel_fraction_max     0.225
_reflns_number_gt                4353
_reflns_number_total             4739
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc05378k2.cif
_cod_data_source_block           bai66cult
_cod_depositor_comments
'Adding full bibliography for 1568013--1568015.cif.'
_cod_original_cell_volume        3745.08(9)
_cod_database_code               1568015
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Re P2 Cl2 C42 H45'
_reflns_odcompleteness_completeness 98.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
3.a Ternary CH refined with riding coordinates:
 C10(H10), C20(H20)
3.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C23(H23), C24(H24),
 C25(H25), C26(H26), C27(H27), 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)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              26084
_shelx_hkl_checksum              43756
_olex2_date_sample_data_collection 2017-03-07
_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 1.409
_oxdiff_exptl_absorpt_empirical_full_min 0.866