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_7061396
_publ_section_title
;
 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         'C37 H36 B Cl Fe Mn N15, C3 H7 N O'
_chemical_formula_sum            'C40 H43 B Cl Fe Mn N16 O'
_chemical_formula_weight         920.95
_chemical_name_systematic        MnL2
_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             2022-03-19
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-03-18 deposited with the CCDC.	2022-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                89.260(5)
_cell_angle_beta                 77.669(5)
_cell_angle_gamma                74.667(5)
_cell_formula_units_Z            2
_cell_length_a                   12.732(2)
_cell_length_b                   13.303(3)
_cell_length_c                   13.725(3)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.52
_cell_volume                     2187.8(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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 7.9580
_diffrn_measured_fraction_theta_full 0.998
_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  0.0539
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            44806
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.365
_diffrn_reflns_theta_min         2.319
_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    0.734
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6824
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1242 before and 0.0643 after correction.
The Ratio of minimum to maximum transmission is 0.9151.
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    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_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   0.682
_refine_diff_density_max         0.971
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         10890
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0374P)^2^+2.1220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1063
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8668
_reflns_number_total             10890
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj00126h2.cif
_cod_data_source_block           Complex2
_cod_depositor_comments
'Adding full bibliography for 7061395--7061398.cif.'
_cod_original_cell_volume        2187.8(7)
_cod_database_code               7061396
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.867
_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. Restrained distances
 O1-C40 \\sim O1A-C40A
 with sigma of 0.02
 N16-C38 \\sim N16-C39A
 with sigma of 0.02
 O1-N16 \\sim O1A-N16
 with sigma of 0.04
 N16-C40 \\sim N16-C40A
 with sigma of 0.02
 N16-C39 \\sim N16-C38A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C38A \\sim C40A \\sim N16 \\sim O1A \\sim C39A: within 2A with sigma of 0.001
and sigma for terminal atoms of 0.002 within 2A
Uanis(C38) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O1(0.8) C40(0.8) H40(0.8) C39(0.8) H39A(0.8) H39B(0.8) H39C(0.8)
 C38(0.8) H38A(0.8) H38B(0.8) H38C(0.8) C39A(0.2) H39D(0.2) H39E(0.2) H39F(0.2)
 O1A(0.2) C40A(0.2) H40A(0.2) C38A(0.2) H38D(0.2) H38E(0.2) H38F(0.2)
5.a Ternary CH refined with riding coordinates:
 B1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C8(H8A,H8B), C7(H7A,H7B), C6(H6A,H6B)
5.c Aromatic/amide H refined with riding coordinates:
 C37(H37), C35(H35), C15(H15), C14(H14), C36(H36), C32(H32), C31(H31),
 C29(H29), C24(H24), C34(H34), C30(H30), C33(H33), C13(H13), C23(H23), C12(H12),
  C4(H4), C22(H22), C21(H21), C1(H1A), C3(H3), C2(H2), C40(H40), C40A(H40A)
5.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C19(H19A,H19B,H19C), C39(H39A,H39B,H39C), C38(H38A,H38B,
 H38C), C39A(H39D,H39E,H39F), C38A(H38D,H38E,H38F)
;
_shelx_res_checksum              58988
_olex2_submission_special_instructions 'No special instructions were received'