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_7135188
_publ_section_title
;
 Synthesis and characterization of rhena-phenalenyl complexes.
;
_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         'C40 H33 Cl2 O2 P2 Re, C H2 Cl2'
_chemical_formula_sum            'C41 H35 Cl4 O2 P2 Re'
_chemical_formula_weight         949.63
_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             2024-11-14
_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                 95.6770(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6366(4)
_cell_length_b                   10.6140(3)
_cell_length_c                   28.7173(9)
_cell_measurement_reflns_used    9831
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      27.59
_cell_measurement_theta_min      2.51
_cell_volume                     3832.8(2)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0490
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            35245
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.704
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.568
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4526
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1964 before and 0.0915 after correction.
The Ratio of minimum to maximum transmission is 0.6070.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         6752
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0225
_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^)+(0.0192P)^2^+1.6059P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0462
_refine_ls_wR_factor_ref         0.0483
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5898
_reflns_number_total             6752
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03639a2.cif
_cod_data_source_block           123
_cod_database_code               7135188
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.740
_shelx_estimated_absorpt_t_min   0.654
_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.a Ternary CH refined with riding coordinates:
 C00C(H00C)
2.b Secondary CH2 refined with riding coordinates:
 C01D(H01D,H01G)
2.c Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00F(H00F), C00K(H00K), C00M(H00M), C00Q(H00Q), C00R(H00R),
 C00S(H00S), C00T(H00T), C00U(H00U), C00W(H00W), C00Z(H00Z), C010(H010),
 C011(H011), C012(H012), C013(H013), C014(H014), C015(H015), C016(H016),
 C017(H017), C018(H018), C019(H019), C01A(H01A), C01B(H01B), C01C(H01C),
 C01E(H01E), C01F(H01F)
2.d Idealised Me refined as rotating group:
 C00V(H00A,H00B,H00E), C00X(H00G,H00H,H00I)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 82 electrons were 
found in a volume of 252\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.5[CH2Cl2] per Asymmetric Unit 
which account for 84 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              83966
_shelx_hkl_checksum              73225
_shelx_fab_checksum              66925
_olex2_submission_special_instructions 'No special instructions were received'