Heterobimetallic cyanide-bridged FeIII(μ-CN)MII complexes (M = Mn and Cu): synthesis, structure and magnetism
Ahmed, Sayeed; Kumar, Akhilesh; Mukhopadhyay, Narottam; Lloret, Francesc; Mukherjee, Rabindranath; New Journal of Chemistry 46 (2022) 7711–7720; doi:10.1039/D2NJ00126H

data_7061398
_publ_section_title
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 Heterobimetallic cyanide-bridged FeIII(\m-CN)MII complexes (M = Mn and
 Cu): synthesis, structure and magnetism
;
_journal_issue                   16
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7711
_journal_page_last               7720
_journal_paper_doi               10.1039/D2NJ00126H
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C36 H34 B Cl Fe Mn N15, 3[C3H7NO], 3[H2O] '
_chemical_formula_sum            'C45 H61 B Cl Fe Mn N18 O6'
_chemical_formula_weight         1107.16
_chemical_name_systematic        MnL1
_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             2022-03-13
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-03-12 deposited with the CCDC.	2022-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                69.201(5)
_cell_angle_beta                 75.879(6)
_cell_angle_gamma                78.786(5)
_cell_formula_units_Z            2
_cell_length_a                   9.4725(18)
_cell_length_b                   16.045(3)
_cell_length_c                   17.654(3)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.34
_cell_volume                     2415.2(8)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 7.9580
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38602
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.311
_diffrn_reflns_theta_min         2.615
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.687
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6644
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1465 before and 0.0593 after correction.
The Ratio of minimum to maximum transmission is 0.8910.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear orangish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1156
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.746
_exptl_transmission_factor_min   0.664
_refine_diff_density_max         1.416
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         11971
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0590P)^2^+1.7726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1312
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9603
_reflns_number_total             11971
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj00126h2.cif
_cod_data_source_block           Complex1
_cod_depositor_comments
'Adding full bibliography for 7061395--7061398.cif.'
_cod_original_cell_volume        2415.1(8)
_cod_database_code               7061398
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.875
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 N1, C1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Fixed Sof: Cl1(0.93) Cl1A(0.07)
4.a Ternary CH refined with riding coordinates:
 B1(H1A)
4.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C6(H6A,H6B), C7(H7A,H7B)
4.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C28(H28), C36(H36), C30(H30), C29(H29), C21(H21), C33(H33),
 C34(H34), C22(H22), C31(H31), C4(H4), C35(H35), C23(H23), C1(H1), C2(H2),
 C32(H32), C3(H3), C14(H14), C11(H11), C13(H13), C12(H12)
4.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C9(H9A,H9B,H9C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 316 electrons were 
found in a volume of 747\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
3[C3H7NO], 3[H2O] per Formula Unit 
which account for 300 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              75339
_shelx_fab_checksum              25630
_olex2_submission_special_instructions 'No special instructions were received'