Acid-responsive rhenium(I) NHC complexes: pyrazine <i>vs.</i> pyridine.
Abate, Pedro O.; Rizo, José Francisco; Fernández-de-Córdova, Francisco José; Ros, Abel; Rivada-Wheelaghan, Orestes; Dalton transactions (Cambridge, England : 2003) 55 (2026) 4677–4686; doi:10.1039/d6dt00158k

data_7720280
_publ_section_title
;
 Acid-responsive rhenium(I) NHC complexes: pyrazine <i>vs.</i> pyridine.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4677
_journal_page_last               4686
_journal_paper_doi               10.1039/d6dt00158k
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C23 H22 N4 O3 Re, F6 P, 2(C7 H8)'
_chemical_formula_sum            'C37 H38 F6 N4 O3 P Re'
_chemical_formula_weight         917.88
_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     dual
_audit_creation_date             2025-04-25
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-12-16 deposited with the CCDC.	2026-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                72.895(2)
_cell_angle_beta                 87.830(2)
_cell_angle_gamma                84.825(2)
_cell_formula_units_Z            4
_cell_length_a                   11.1996(6)
_cell_length_b                   15.6853(8)
_cell_length_c                   22.5574(11)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      28.025
_cell_measurement_theta_min      2.368
_cell_volume                     3771.7(3)
_computing_cell_refinement       'SAINT V8.41 (Bruker AXS LLC)'
_computing_data_reduction        'SAINT V8.41 (Bruker AXS LLC)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.00
_diffrn_detector                 'Bruker Photon II area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1283
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            108223
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         1.826
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    3.335
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0923 before and 0.0762 after correction.
The Ratio of minimum to maximum transmission is 0.8599.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       plate
_exptl_crystal_F_000             1824
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene - CH3CN'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.096
_refine_diff_density_min         -2.171
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     949
_refine_ls_number_reflns         14335
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0211P)^2^+26.8380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1157
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11026
_reflns_number_total             14335
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00158k3.cif
_cod_data_source_block           orw0925a
_cod_depositor_comments
'Adding full bibliography for 7720278--7720280.cif.'
_cod_database_code               7720280
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.732
_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
 C30C-C24C
 1.51 with sigma of 0.02
 C24C-C25C = C24C-C29C = C26C-C27C
 1.39 with sigma of 0.02
 C25C-C26C = C27C-C28C = C28C-C29C
 1.38 with sigma of 0.02
 C30C-C25C = C30C-C29C
 2.52 with sigma of 0.04
 C24C-C26C
 2.42 with sigma of 0.04
 C24C-C28C
 2.41 with sigma of 0.04
 C25C-C27C
 2.39 with sigma of 0.04
 C26C-C28C = C27C-C29C
 2.4 with sigma of 0.04
 C24C-C25C \\sim C25C-C26C \\sim C26C-C27C \\sim C27C-C28C \\sim C28C-C29C
\\sim C29C-C24C
 with sigma of 0.02
 C24C-C28C \\sim C24C-C26C \\sim C29C-C27C \\sim C25C-C29C \\sim C26C-C28C
\\sim C25C-C27C
 with sigma of 0.04
 C30C-C29C \\sim C30C-C25C
 with sigma of 0.04
3. Restrained planarity
 C24C, C25C, C26C, C27C, C28C, C29C, C30C
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C24C \\sim C25C \\sim C26C \\sim C27C \\sim C28C \\sim C29C \\sim C30C: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C24C, C25C, C26C, C27C, C28C, C29C, C30C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C6A(H6AA,H6AB)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C12(H12), C14(H14), C1A(H1A),
 C2A(H2A), C3A(H3A), C4A(H4A), C8A(H8A), C9A(H9A), C12A(H12A), C14A(H14A),
 C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C25B(H25B), C26B(H26B),
 C27B(H27B), C28B(H28B), C29B(H29B), C25A(H25A), C26A(H26A), C27A(H27A),
 C28A(H28A), C29A(H29A), C25C(H25C), C26C(H26C), C27C(H27C), C28C(H28C),
 C29C(H29C)
6.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C23(H23A,H23B,
 H23C), C16A(H16D,H16E,H16F), C17A(H17D,H17E,H17F), C18A(H18D,H18E,H18F),
 C23A(H23D,H23E,H23F), C30(H30A,H30B,H30C), C30B(H30D,H30E,H30F), C30A(H30G,
 H30H,H30I), C30C(H30J,H30K,H30L)
;
_shelx_res_checksum              92170
_shelx_hkl_checksum              14126
_olex2_submission_special_instructions 'No special instructions were received'