Radical metallacyclopropene: synthesis, structure and aromaticity
Bai, Wei; Li, Lei; Fu, Yukang; Tang, Junping; Zhao, Yue; Wang, Yilun; Yang, Li; Dalton Transactions  (2023) –; doi:10.1039/D3DT01558K

data_7713288
_publ_section_title
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 Radical metallacyclopropene: synthesis, structure and aromaticity
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01558K
_journal_year                    2023
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C34 H31 Cl3 O P2 Re'
_chemical_formula_sum            'C34 H31 Cl3 O P2 Re'
_chemical_formula_weight         810.08
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-12
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
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_audit_update_record
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2023-06-14 deposited with the CCDC.	2023-06-27 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0621(2)
_cell_length_b                   18.0532(4)
_cell_length_c                   18.0532(4)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      26.366
_cell_measurement_theta_min      2.159
_cell_volume                     3605.34(13)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40698
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.366
_diffrn_reflns_theta_min         2.159
_exptl_absorpt_coefficient_mu    3.705
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0105
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0794 before and 0.0601 after correction.
The Ratio of minimum to maximum transmission is 0.3804.
The \l/2 correction factor is Not present.
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_exptl_crystal_colour            'metallic blackish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       block
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
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_refine_ls_abs_structure_Flack   0.082(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         7399
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0409P)^2^+0.7687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0748
_reflns_Friedel_coverage         0.791
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6782
_reflns_number_total             7399
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01558k2.cif
_cod_data_source_block           1
_cod_database_code               7713288
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.708
_shelx_estimated_absorpt_t_min   0.708
_olex2_refinement_description
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1. Twinned data refinement
 Scales: 0.918(8)
 0.082(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
4.a Ternary CH refined with riding coordinates:
 C8(H8)
4.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C30(H30), C27(H27), C10(H10), C12(H12), C14(H14), C4(H4), C11(H11),
 C19(H19), C7(H7), C31(H31), C26(H26), C13(H13), C33(H33), C34(H34), C5(H5),
 C6(H6), C32(H32), C16(H16), C24(H24), C17(H17), C18(H18), C28(H28), C25(H25)
4.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
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_smtbx_masks_special_details
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A solvent mask was calculated and 126 electrons were 
found in a volume of 758\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.8[C4H8O] per Asymmetric Unit 
which account for 128 electrons 
per unit cell.
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_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              78157
_shelx_fab_checksum              35025
_olex2_submission_special_instructions 'No special instructions were received'