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_7061397
_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         'C36 H34 B Cu Fe N15, Cl O4, 2[CH4O]'
_chemical_formula_sum            'C38 H42 B Cl Cu Fe N15 O6'
_chemical_formula_weight         970.51
_chemical_name_systematic        CuL1
_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             2022-03-16
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-03-16 deposited with the CCDC.	2022-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                71.814(9)
_cell_angle_beta                 69.341(9)
_cell_angle_gamma                86.686(9)
_cell_formula_units_Z            2
_cell_length_a                   12.941(5)
_cell_length_b                   13.510(6)
_cell_length_c                   13.967(6)
_cell_measurement_reflns_used    7110
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.048
_cell_measurement_theta_min      2.189
_cell_volume                     2167.0(16)
_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_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  0.0616
_diffrn_reflns_av_unetI/netI     0.0745
_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       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20815
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.048
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_min         2.189
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.951
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4697
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1528 before and 0.0651 after correction.
The Ratio of minimum to maximum transmission is 0.6299.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear brownish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeOH'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   0.746
_exptl_transmission_factor_min   0.470
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         7670
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0531
_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^)+(0.0613P)^2^+1.5688P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1296
_refine_ls_wR_factor_ref         0.1440
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5601
_reflns_number_total             7670
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj00126h2.cif
_cod_data_source_block           Complex3
_cod_depositor_comments
'Adding full bibliography for 7061395--7061398.cif.'
_cod_original_cell_volume        2167.1(16)
_cod_database_code               7061397
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.945
_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
 Cl1-O3 \\sim Cl1A-O3A
 with sigma of 0.02
 O3-O1 \\sim O3A-O1A
 with sigma of 0.04
 Cl1-O4 \\sim Cl1A-O4A
 with sigma of 0.02
 O4-O2 \\sim O4A-O2A
 with sigma of 0.04
 Cl1-O2 \\sim Cl1A-O2A
 with sigma of 0.02
 Cl1-O1 \\sim Cl1A-O1A
 with sigma of 0.02
 O4-O1 \\sim O4A-O1A
 with sigma of 0.04
 O2-O1 \\sim O2A-O1A
 with sigma of 0.04
 O3-O4 \\sim O3A-O4A
 with sigma of 0.04
 O3-O2 \\sim O3A-O2A
 with sigma of 0.04
3. Rigid bond restraints
 C19, C24
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
O2 \\sim O4 \\sim Cl1 \\sim O1 \\sim O3: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
O4A \\sim O3A \\sim O2A \\sim O1A \\sim Cl1A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
5. Others
 Sof(Cu1A)=1-FVAR(1)
 Sof(Cu1)=FVAR(1)
 Fixed Sof: Cl1(0.65) O3(0.65) O4(0.65) O2(0.65) O1(0.65) O2A(0.35) Cl1A(0.35)
 O3A(0.35) O4A(0.35) O1A(0.35)
6.a Ternary CH refined with riding coordinates:
 B1(H1A)
6.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C16(H16A,H16B), C7(H7A,H7B)
6.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C34(H34), C28(H28), C36(H36), C31(H31), C2(H2), C1(H1), C35(H35),
 C32(H32), C4(H4), C22(H22), C30(H30), C29(H29), C3(H3), C20(H20), C21(H21),
 C33(H33), C14(H14), C11(H11), C12(H12), C13(H13)
6.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 82 electrons were 
found in a volume of 252\%A^3^ in one void per unit cell. 
This is consistent with the presence of 
2[CH3OH] per Formula Unit 
which account for 72 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              68398
_shelx_fab_checksum              46885
_olex2_submission_special_instructions 'No special instructions were received'