Synthesis, Structure and Aromaticity of Metallapyridinium Complexes
Wang, Yilun; Sun, Yue; Bai, Wei; Zhou, Yan; Bao, Xiao; Yang, Li; Dalton Transactions  (2022) –; doi:10.1039/D1DT04096K

data_7709309
_publ_section_title
;
 Synthesis, Structure and Aromaticity of Metallapyridinium Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04096K
_journal_year                    2022
_chemical_formula_moiety         'C48 H45 Cl3 N P3 Re, C3 H6 O, C24 H20 B'
_chemical_formula_sum            'C75 H71 B Cl3 N O P3 Re'
_chemical_formula_weight         1398.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_audit_creation_date             2021-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-24 deposited with the CCDC.	2022-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.1640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2784(8)
_cell_length_b                   22.0302(9)
_cell_length_c                   17.0720(7)
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      24.16
_cell_measurement_theta_min      2.39
_cell_volume                     6964.0(5)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      190.0
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_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  0.1040
_diffrn_reflns_av_unetI/netI     0.1068
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            60184
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         2.227
_exptl_absorpt_coefficient_mu    1.972
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.629
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       block
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.260
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     813
_refine_ls_number_reflns         15113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0507
_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^)+(0.0479P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1156
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9416
_reflns_number_total             15113
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04096k2.cif
_cod_data_source_block           baiwei12
_cod_database_code               7709309
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.827
_shelx_estimated_absorpt_t_min   0.545
_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. Others
 Fixed Sof: O1S(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5) C2S(0.5) C3S(0.5)
 H3SA(0.5) H3SB(0.5) H3SC(0.5) O2S(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5) H4SC(0.5)
 C5S(0.5) C6S(0.5) H6SA(0.5) H6SB(0.5) H6SC(0.5)
3.a Ternary CH refined with riding coordinates:
 C1(H1A)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C24(H24), C25(H25),
  C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33), C34(H34),
 C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C43(H43), C44(H44),
  C45(H45), C46(H46), C47(H47), C50(H50), C51(H51), C52(H52), C53(H53),
 C54(H54), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60), C62(H62), C63(H63),
  C64(H64), C65(H65), C66(H66), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72)
3.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C29(H29A,H29B,H29C), C48(H48A,H48B,H48C), C1S(H1SA,H1SB,
 H1SC), C3S(H3SA,H3SB,H3SC), C4S(H4SA,H4SB,H4SC), C6S(H6SA,H6SB,H6SC)
;
_shelx_res_checksum              61345
_olex2_submission_special_instructions 'No special instructions were received'