Observation of protonation-induced intra-molecular metal-to-metal charge transfer in cyano-bridged [Fe−CN−Mn/Ni] dinuclear complexes
Jia, Shuwen; Zhu, Xinrui; Li, Dongfeng; Dalton Transactions  (2023) –; doi:10.1039/D3DT02200E

data_7713978
_publ_section_title
;
 Observation of protonation-induced intra-molecular metal-to-metal charge
 transfer in cyano-bridged [Fe&#x2212;CN&#x2212;Mn/Ni] dinuclear complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02200E
_journal_year                    2023
_chemical_formula_moiety         'C29 H26 N5 Ni O, 2(Cl O4)'
_chemical_formula_sum            'C29 H26 Cl2 N5 Ni O9'
_chemical_formula_weight         718.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-04-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-04-20 deposited with the CCDC.	2023-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 120.023(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.388(4)
_cell_length_b                   12.490(2)
_cell_length_c                   12.860(2)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      62.31
_cell_measurement_theta_min      3.71
_cell_volume                     2974.4(9)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip  (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22182
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         62.316
_diffrn_reflns_theta_min         3.714
_diffrn_source_current           3.58
_diffrn_source_power             0.250421
_diffrn_source_voltage           69.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.019
_exptl_absorpt_correction_T_max  0.7521
_exptl_absorpt_correction_T_min  0.3858
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1608 before and 0.0852 after correction.
The Ratio of minimum to maximum transmission is 0.5130.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       block
_exptl_crystal_F_000             1476
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0790P)^2^+2.1857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1236
_refine_ls_wR_factor_ref         0.1300
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3056
_reflns_number_total             3582
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02200e2.cif
_cod_data_source_block           230329l-1
_cod_database_code               7713978
_shelx_shelxl_version_number     2018/3
_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, All O(H) groups
2. Others
 Fixed Sof: H1(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C2(H2), C4(H4), C12(H12), C10(H10), C13(H13), C1(H1A), C3(H3),
 C14(H14), C9(H9)
3.b Tetrahedral OH refined with riding coordinates:
 O1(H1)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_shelx_res_checksum              49503
_olex2_submission_special_instructions 'No special instructions were received'