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_7713979
_publ_section_title
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 Observation of protonation-induced intra-molecular metal-to-metal charge
 transfer in cyano-bridged [Fe&#x2212;CN&#x2212;Mn/Ni] dinuclear complexes
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02200E
_journal_year                    2023
_chemical_formula_moiety         'C51 H36 Fe N13 Ni'
_chemical_formula_sum            'C51 H36 Fe N13 Ni'
_chemical_formula_weight         945.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-04-19
_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                 102.266(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4824(11)
_cell_length_b                   14.1597(12)
_cell_length_c                   25.064(2)
_cell_measurement_reflns_used    9072
_cell_measurement_temperature    100
_cell_measurement_theta_max      53.02
_cell_measurement_theta_min      2.92
_cell_volume                     4675.7(7)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.995
_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  0.0894
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            62227
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.096
_diffrn_reflns_theta_max         53.096
_diffrn_reflns_theta_min         2.918
_diffrn_source_current           3.57
_diffrn_source_power             0.2497215
_diffrn_source_voltage           69.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.179
_exptl_absorpt_correction_T_max  0.7505
_exptl_absorpt_correction_T_min  0.3916
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1555 before and 0.0840 after correction.
The Ratio of minimum to maximum transmission is 0.5218.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       block
_exptl_crystal_F_000             1948
_refine_diff_density_max         0.959
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         8249
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0724
_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^)+(0.0492P)^2^+26.7369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1752
_refine_ls_wR_factor_ref         0.1822
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6592
_reflns_number_total             8249
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02200e2.cif
_cod_data_source_block           230329n-1_a_sq
_cod_database_code               7713979
_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
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14), C19(H19),
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C31(H31),
  C32(H32), C33(H33), C38(H38), C39(H39), C40(H40), C41(H41), C43(H43),
 C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50)
2.b Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              39807
_shelx_fab_checksum              74745
_platon_squeeze_special_details
;
A solvent mask was calculated and 184 electrons were 
found in a volume of 688\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
1.5[CH3OH], 1[CH3OH] per Asymmetric Unit 
which account for 180 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'