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_7713977
_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 Mn N5 O, 2(Cl O4)'
_chemical_formula_sum            'C29 H26 Cl2 Mn N5 O9'
_chemical_formula_weight         714.39
_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
_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                 120.374(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.6669(17)
_cell_length_b                   12.5249(11)
_cell_length_c                   12.9279(11)
_cell_measurement_reflns_used    8050
_cell_measurement_temperature    100
_cell_measurement_theta_max      55.50
_cell_measurement_theta_min      3.70
_cell_volume                     3026.8(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker Photon III 28 detector'
_diffrn_detector_area_resol_mean ' 7.39 for PHOTON III'
_diffrn_detector_type            'Bruker Photon III 28'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker D8 Venture'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Metaljet Helios MX'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     1.34139
_diffrn_radiation_xray_symbol    'Ga K\a'
_diffrn_reflns_av_R_equivalents  0.0996
_diffrn_reflns_av_unetI/netI     0.0628
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16648
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        52.096
_diffrn_reflns_theta_max         52.096
_diffrn_reflns_theta_min         3.696
_diffrn_source                   'METALJET liquid metal X-ray source'
_diffrn_source_current           3.57
_diffrn_source_power             0.2497215
_diffrn_source_target            Ga
_diffrn_source_type              'Sealed X-ray tube'
_diffrn_source_voltage           69.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.871
_exptl_absorpt_correction_T_max  0.7510
_exptl_absorpt_correction_T_min  0.2495
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1768 before and 0.1117 after correction.
The Ratio of minimum to maximum transmission is 0.3322.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_refine_diff_density_max         0.903
_refine_diff_density_min         -1.652
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         2580
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.229
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0830
_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^)+(0.1867P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2294
_refine_ls_wR_factor_ref         0.2473
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2148
_reflns_number_total             2580
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02200e2.cif
_cod_data_source_block           230329k-1_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_database_code               7713977
_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. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N3) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(Mn1) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: H1(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C1(H1A), C13(H13), C2(H2), C4(H4), C9(H9), C15(H15), C14(H14),
 C3(H3), C10(H10)
4.b Tetrahedral OH refined with riding coordinates:
 O1(H1)
4.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_shelx_res_checksum              6891
_olex2_submission_special_instructions 'No special instructions were received'