Aza-metallacycles with a heptavalent Re (d<sup>0</sup>) center.
Wang, Qianhang; Wang, Yarong; Zhao, Yue; Li, Yang; Jiang, Wenfeng; Bai, Wei; Dalton transactions (Cambridge, England : 2003) 53 (2024) 12872–12875; doi:10.1039/d4dt02082k

data_7716704
_publ_section_title
;
 Aza-metallacycles with a heptavalent Re (d<sup>0</sup>) center.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12872
_journal_page_last               12875
_journal_paper_doi               10.1039/d4dt02082k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C27 H24 Cl3 N O P Re, 1.5[CH2Cl2]'
_chemical_formula_sum            'C28.5 H27 Cl6 N O P Re'
_chemical_formula_weight         829.38
_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             2023-07-25
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-04-16 deposited with the CCDC.	2024-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.990(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4425(6)
_cell_length_b                   22.9633(12)
_cell_length_c                   14.0700(8)
_cell_measurement_reflns_used    4282
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      23.90
_cell_measurement_theta_min      2.30
_cell_volume                     3170.6(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0978
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            54895
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.023
_diffrn_reflns_theta_max         25.023
_diffrn_reflns_theta_min         2.257
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    4.412
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0992 before and 0.0788 after correction.
The Ratio of minimum to maximum transmission is 0.3696.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_description       block
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.636
_refine_diff_density_min         -1.884
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5588
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0331P)^2^+9.1683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.0993
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4511
_reflns_number_total             5588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02082k3.cif
_cod_data_source_block           1_sq
_cod_depositor_comments
'Adding full bibliography for 7716703--7716704.cif.'
_cod_original_formula_sum        'C28.50 H27 Cl6 N O P Re'
_cod_database_code               7716704
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.667
_shelx_estimated_absorpt_t_min   0.557
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
C25 \\sim C23 \\sim C22 \\sim C26 \\sim C24 \\sim C27: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01 within 2A
C7 \\sim C8 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.001 within 2A
C26 \\sim C25 \\sim C24 \\sim C23 \\sim C22 \\sim C27: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01 within 2A
C25 \\sim C24 \\sim C23 \\sim C22 \\sim C27 \\sim C26: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01 within 2A
2. Rigid body (RIGU) restrains
 C25, C26, C27, C22, C23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C7(H7), C5(H5), C8(H8), C15(H15), C17(H17), C23(H23), C20(H20),
 C11(H11), C13(H13), C21(H21), C14(H14), C27(H27), C18(H18), C26(H26), C24(H24),
  C25(H25), C19(H19), C12(H12)
3.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C)
;
_shelx_res_checksum              73460
_shelx_hkl_checksum              1878
_shelx_fab_checksum              8618
_platon_squeeze_special_details
;
A solvent mask was calculated and 245 electrons were 
found in a volume of 720\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1.5[CH2Cl2] per Asymmetric Unit 
which account for 252 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'