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_7061395
_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 Cu Fe N15, Cl O4, C2 H3 N, 1[C2H3N]'
_chemical_formula_sum            'C41 H42 B Cl Cu Fe N17 O4'
_chemical_formula_weight         1002.56
_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             2021-12-17
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2021-12-17 deposited with the CCDC.	2022-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                106.8250(10)
_cell_angle_beta                 93.9980(10)
_cell_angle_gamma                109.8850(10)
_cell_formula_units_Z            2
_cell_length_a                   12.8584(5)
_cell_length_b                   13.2149(6)
_cell_length_c                   15.1082(6)
_cell_measurement_reflns_used    9250
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.43
_cell_volume                     2270.13(16)
_computing_cell_refinement       '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_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0478
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28294
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.049
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_min         2.552
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.909
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6818
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1399 before and 0.0578 after correction.
The Ratio of minimum to maximum transmission is 0.9143.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear reddish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         8022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0544P)^2^+2.2446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1167
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6428
_reflns_number_total             8022
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj00126h2.cif
_cod_data_source_block           Complex4
_cod_depositor_comments
'Adding full bibliography for 7061395--7061398.cif.'
_cod_original_cell_volume        2270.12(16)
_cod_database_code               7061395
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.839
_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.a Ternary CH refined with riding coordinates:
 B1(H1A)
2.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C16(H16A,H16B), C6(H6A,H6B), C7(H7A,H7B)
2.c Aromatic/amide H refined with riding coordinates:
 C33(H33), C34(H34), C29(H29), C31(H31), C32(H32), C30(H30), C37(H37),
 C24(H24), C36(H36), C35(H35), C21(H21), C23(H23), C9(H9), C2(H2), C1(H1),
 C22(H22), C4(H4), C12(H12), C3(H3), C10(H10), C11(H11)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C19(H19A,H19B,H19C), C38(H38A,H38B,H38C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 49 electrons were 
found in a volume of 244\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[C2H3N] per Unit Cell 
which account for 44 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              95946
_shelx_fab_checksum              35014
_olex2_submission_special_instructions 'No special instructions were received'