An aromatic dimetallapolycyclic complex with two rhenapyrylium rings
Bai, Wei; Sun, Yue; Wang, Yilun; Zhou, Yan; Zhao, Yue; Bao, Xiao; Yang, Li; Chemical Communications  (2022) –; doi:10.1039/D2CC01789J

data_7130034
_publ_section_title
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 An aromatic dimetallapolycyclic complex with two rhenapyrylium rings
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC01789J
_journal_year                    2022
_chemical_formula_moiety         'C39 H34 Cl3 O P2 Re, C H2 Cl2'
_chemical_formula_sum            'C40 H36 Cl5 O P2 Re'
_chemical_formula_weight         958.08
_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
_audit_creation_date             2022-04-23
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-04-24 deposited with the CCDC.	2022-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                97.1060(10)
_cell_angle_beta                 96.7000(10)
_cell_angle_gamma                102.4130(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3695(6)
_cell_length_b                   12.1973(8)
_cell_length_c                   16.6779(10)
_cell_measurement_reflns_used    9669
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.28
_cell_volume                     2021.8(2)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.00
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.990
_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  0.0283
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            53167
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         3.242
_exptl_absorpt_coefficient_mu    3.445
_exptl_absorpt_correction_T_max  0.716
_exptl_absorpt_correction_T_min  0.709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       block
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.964
_refine_diff_density_min         -1.274
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         8752
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0243
_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^)+(0.0304P)^2^+5.5497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0623
_refine_ls_wR_factor_ref         0.0628
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8491
_reflns_number_total             8752
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01789j2.cif
_cod_data_source_block           baiwei26
_cod_database_code               7130034
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C41) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C40) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: Cl4(0.5) Cl5(0.5) C40(0.5) H40A(0.5) H40B(0.5) Cl6(0.5) Cl7(0.5)
 C41(0.5) H41A(0.5) H41B(0.5)
4.a Ternary CH refined with riding coordinates:
 C1(H1)
4.b Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C41(H41A,H41B)
4.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25),
  C26(H26), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C35(H35),
 C36(H36), C37(H37), C38(H38), C39(H39)
4.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              79209
_shelx_hkl_checksum              48520
_olex2_submission_special_instructions 'No special instructions were received'