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_7713289
_publ_section_title
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 Radical metallacyclopropene: synthesis, structure and aromaticity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01558K
_journal_year                    2023
_chemical_formula_moiety         'C34 H31 Cl2 O2 P2 Re'
_chemical_formula_sum            'C34 H31 Cl2 O2 P2 Re'
_chemical_formula_weight         790.63
_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             2023-06-12
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_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                107.3720(10)
_cell_angle_beta                 92.398(2)
_cell_angle_gamma                106.532(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5704(4)
_cell_length_b                   11.4035(5)
_cell_length_c                   13.9505(6)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      57.014
_cell_measurement_theta_min      3.719
_cell_volume                     1523.69(11)
_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 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17755
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.414
_diffrn_reflns_theta_min         1.544
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    4.299
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            'metallic bluish blue'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_description       noodle
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.518
_refine_diff_density_min         -2.040
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         6197
_refine_ls_number_restraints     691
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+6.5948P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.0992
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5674
_reflns_number_total             6197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01558k2.cif
_cod_data_source_block           1_CCDC1
_cod_database_code               7713289
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.919
_shelx_estimated_absorpt_t_min   0.673
_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. Rigid bond restraints
 Re1, P1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
C1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
Re1 \\sim P1: within 2A with sigma of 0.007 and sigma for terminal atoms of
0.001 within 2A
C10 \\sim C1 \\sim C3 \\sim C2 \\sim C11 \\sim C15 \\sim C8 \\sim C23 \\sim C29
\\sim C16 \\sim C7 \\sim C25 \\sim C5 \\sim C9 \\sim C12 \\sim C4 \\sim C22
\\sim C28 \\sim C19 \\sim C24 \\sim C20 \\sim C14 \\sim C6 \\sim C18 \\sim C13
\\sim C26 \\sim C17 \\sim C30 \\sim C27 \\sim C34 \\sim C21 \\sim C32 \\sim C33
\\sim C31: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 3.8A
Uanis(P2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
4. Rigid body (RIGU) restrains
 P1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C15(H15), C8(H8), C7(H7), C25(H25), C5(H5), C12(H12), C4(H4),
 C28(H28), C19(H19), C24(H24), C20(H20), C14(H14), C6(H6), C18(H18), C13(H13),
 C26(H26), C17(H17), C30(H30), C27(H27), C34(H34), C21(H21), C32(H32), C33(H33),
  C31(H31)
5.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C22(H22A,H22B,H22C)
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_shelx_res_checksum              63923
_olex2_submission_special_instructions 'No special instructions were received'