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_7130033
_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
'C33 H31 Cl3 O P2 Re, C33 H29 Cl3 O P2 Re, C3 H7, C H2 Cl2, [+ solvents]'
_chemical_formula_sum            'C70 H69 Cl8 O2 P4 Re2'
_chemical_formula_weight         1722.13
_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     iterative
_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
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2022-04-24 deposited with the CCDC.	2022-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                87.311(4)
_cell_angle_beta                 88.052(4)
_cell_angle_gamma                83.508(4)
_cell_formula_units_Z            2
_cell_length_a                   13.5626(6)
_cell_length_b                   16.9269(8)
_cell_length_c                   17.6821(8)
_cell_measurement_reflns_used    33288
_cell_measurement_temperature    120
_cell_measurement_theta_max      66.596
_cell_measurement_theta_min      3.709
_cell_volume                     4027.2(3)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1394
_diffrn_reflns_av_unetI/netI     0.1511
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33288
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        66.596
_diffrn_reflns_theta_max         66.596
_diffrn_reflns_theta_min         3.709
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    9.276
_exptl_absorpt_correction_T_max  0.455
_exptl_absorpt_correction_T_min  0.396
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'reddish red'
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       block
_exptl_crystal_F_000             1702
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.622
_refine_diff_density_min         -1.435
_refine_diff_density_rms         0.288
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         13766
_refine_ls_number_restraints     223
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1568
_refine_ls_R_factor_gt           0.1105
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2699
_refine_ls_wR_factor_ref         0.2942
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9638
_reflns_number_total             13766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01789j2.cif
_cod_data_source_block           baiwei25
_cod_database_code               7130033
_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. Restrained distances
 C70_$1-C70
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C70 \\sim C69 \\sim C68: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01 within 2A
C13 \\sim C11 \\sim C10 \\sim C9 \\sim C14 \\sim C12 \\sim C51 \\sim C52 \\sim
C50 \\sim C49 \\sim C53 \\sim C48 \\sim C25 \\sim C24 \\sim C23 \\sim C22 \\sim
C26: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
C39 \\sim C38 \\sim C70 \\sim C69 \\sim C68 \\sim C44 \\sim C45 \\sim C21 \\sim
C32 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C27: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01 within 2A
C68 \\sim C69 \\sim C70 \\sim C67: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 2A
C21 \\sim C7 \\sim C40 \\sim C36 \\sim C37: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.01 within 2A
C16 \\sim C7: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
within 2A
C21: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
C18: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
C70: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
Re2 \\sim Re1: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 2A
Cl8 \\sim Cl7: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 2A
Uanis(C57) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C26) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C58) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(Cl8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C70) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(Re2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C70
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5.a Ternary CH refined with riding coordinates:
 C34(H34), C1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C69(H69A,H69B), C70(H70A,H70B), C67(H67A,H67B)
5.c Aromatic/amide H refined with riding coordinates:
 C40(H40), C47(H47), C43(H43), C44(H44), C45(H45), C46(H46), C49(H49),
 C50(H50), C51(H51), C52(H52), C53(H53), C59(H59), C58(H58), C57(H57), C56(H56),
  C55(H55), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C7(H7), C13(H13),
 C14(H14), C10(H10), C11(H11), C12(H12), C16(H16), C18(H18), C20(H20), C22(H22),
  C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30),
 C31(H31), C32(H32)
5.d Fitted hexagon refined as free rotating group:
 C47(C42,C43,C44,C45,C46), C48(C49,C50,C51,C52,C53), C54(C59,C58,C57,C56,C55),
 C61(C62,C63,C64,C65,C66), C13(C14,C9,C10,C11,C12), C15(C16,C17,C18,C19,C20),
 C22(C23,C24,C25,C26,C21), C27(C28,C29,C30,C31,C32)
5.e Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C60(H60A,H60B,H60C), C6(H6A,H6B,
 H6C), C8(H8A,H8B,H8C), C33(H33A,H33B,H33C), C68(H68A,H68B,H68C)
;
_shelx_res_checksum              42642
_shelx_hkl_checksum              38365
_shelx_fab_checksum              34954
_platon_squeeze_special_details
;
A solvent mask was calculated and 468 electrons were 
found in a volume of 809\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2.5[CH2CL2] per Asymmetric Unit 
which account for 210 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'