One-pot syntheses of rhena-2-benzopyrylium complexes with a fused metallacyclopropene unit.
Bao, Xiao; Li, Yang; Bai, Wei; Zhou, Yan; Wang, Yilun; Sun, Yue; Jiang, Jingyang; Chemical communications (Cambridge, England) 57 (2021) 1643–1646; doi:10.1039/d0cc07749f

data_7127799
_publ_section_title
;
 One-pot syntheses of rhena-2-benzopyrylium complexes with a fused
 metallacyclopropene unit.
;
_journal_issue                   13
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1643
_journal_page_last               1646
_journal_paper_doi               10.1039/d0cc07749f
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C36 H31 Cl3 F3 O P2 Re, C0.5 H Cl'
_chemical_formula_sum            'C36.5 H32 Cl4 F3 O P2 Re'
_chemical_formula_weight         933.56
_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     iterative
_audit_creation_date             2020-10-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-26 deposited with the CCDC.	2021-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.387(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.8031(11)
_cell_length_b                   22.2110(12)
_cell_length_c                   17.0555(9)
_cell_measurement_reflns_used    7613
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.56
_cell_measurement_theta_min      2.67
_cell_volume                     7455.2(7)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0891
_diffrn_reflns_av_unetI/netI     0.0981
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35394
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         2.403
_exptl_absorpt_coefficient_mu    3.676
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_description       block
_exptl_crystal_F_000             3672
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.477
_refine_diff_density_min         -1.593
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         7929
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0636P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1278
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5300
_reflns_number_total             7929
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07749f2.cif
_cod_data_source_block           baiwei5
_cod_depositor_comments
'Adding full bibliography for 7127799--7127800.cif.'
_cod_original_formula_sum        'C36.50 H32 Cl4 F3 O P2 Re'
_cod_database_code               7127799
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.710
_shelx_estimated_absorpt_t_min   0.609
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F2A-F1A
 2 with sigma of 0.02
 F2-F1
 2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F1A) = Uanis(F1)
Uanis(F2) = Uanis(F2A)
Uanis(F3) = Uanis(F3A)
4. Others
 Sof(F1)=Sof(F2A)=Sof(F3A)=1-FVAR(1)
 Sof(F2)=Sof(F3)=Sof(F1A)=FVAR(1)
 Fixed Sof: Cl1S(0.5) C1S(0.5) H1SA(0.32) H1SB(0.32) H1SC(0.18) H1SD(0.18)
 Cl2S(0.32) Cl3S(0.18)
5.a Ternary CH refined with riding coordinates:
 C1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C1S(H1SC,H1SD)
5.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9), C13(H13), C14(H14), C15(H15), C16(H16),
 C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26), C27(H27),
  C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
5.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              95227
_olex2_submission_special_instructions 'No special instructions were received'