Synthesis and characterization of rhena-phenalenyl complexes.
Li, Lei; Fu, Bingjie; Zhao, Yue; Sun, Yue; Li, Yang; Jiang, Wenfeng; Bai, Wei; Chemical communications (Cambridge, England) 61 (2025) 15858–15861; doi:10.1039/d5cc03639a

data_7135187
_publ_section_title
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 Synthesis and characterization of rhena-phenalenyl complexes.
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_journal_issue                   81
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              15858
_journal_page_last               15861
_journal_paper_doi               10.1039/d5cc03639a
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C53 H47 Cl2 P3 Re, C6 H14, O4 Re, C H4 O '
_chemical_formula_sum            'C60 H65 Cl2 O5 P3 Re2'
_chemical_formula_weight         1402.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-04
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-08-04 deposited with the CCDC.	2025-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.177(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2713(6)
_cell_length_b                   15.3656(8)
_cell_length_c                   30.0068(15)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    149.0
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      2.42
_cell_volume                     5613.6(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      149.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            38522
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.491
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.537
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1272 before and 0.0646 after correction.
The Ratio of minimum to maximum transmission is 0.6120.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic orangish orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_description       block
_exptl_crystal_F_000             2776
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.113
_refine_diff_density_min         -1.794
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         9901
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0345P)^2^+32.6679P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1063
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7308
_reflns_number_total             9901
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03639a2.cif
_cod_data_source_block           2
_cod_database_code               7135187
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.713
_shelx_estimated_absorpt_t_min   0.549
_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, All O(H) groups
2. Restrained distances
 C59-C60 = C58-C59 = C58-C57 = C55-C57
 1.56 with sigma of 0.01
 C56-C55
 1.57 with sigma of 0.01
 C59-C60 \\sim C58-C59 \\sim C58-C57 \\sim C55-C57
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C60) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C57)
\\sim Ueq, Uanis(C55) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C56) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C1(H1), C3(H3)
4.b Secondary CH2 refined with riding coordinates:
 C57(H57A,H57B), C59(H59A,H59B), C55(H55A,H55B), C58(H58A,H58B)
4.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C27(H27), C21(H21), C8(H8), C30(H30), C17(H17), C19(H19), C20(H20),
 C44(H44), C53(H53), C12(H12), C23(H23), C49(H49), C14(H14), C25(H25), C34(H34),
  C24(H24), C26(H26), C32(H32), C9(H9), C10(H10), C31(H31), C13(H13), C50(H50),
 C51(H51), C42(H42), C52(H52), C38(H38), C33(H33), C45(H45), C39(H39), C40(H40),
  C36(H36), C37(H37), C47(H47), C46(H46)
4.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C28(H28A,H28B,H28C), C41(H41A,H41B,H41C), C54(H54A,H54B,
 H54C), C60(H60A,H60B,H60C), C56(H56A,H56B,H56C)
4.e Idealised tetrahedral OH refined as rotating group:
 O1(H1A)
;
_shelx_res_checksum              86916
_shelx_hkl_checksum              26801
_olex2_submission_special_instructions 'No special instructions were received'