Experimental and theoretical magnetostructural study on discrete heterometallic cyanide-bridged dinuclear FeIIIMnII and tetranuclear FeIII2CuII2 complexes bearing a tripodal pyrazolyl borate and tetradentate phenolate-based ligands
Kumar, Akhilesh NIDHI; Rajput, Amit; Kaur, Pawanjeet; Verma, Indresh; Erande, Rohan; Javed, Saleem; Kłak, Julia; Alrebei, Shefa F.; Colacio, Enrique; Mota, Antonio J.; Arora, Himanshu; Dalton Transactions  (2023) –; doi:10.1039/D3DT00604B

data_7712881
_publ_section_title
;
 Experimental and theoretical magnetostructural study on discrete
 heterometallic cyanide-bridged dinuclear FeIIIMnII and tetranuclear
 FeIII2CuII2 complexes bearing a tripodal pyrazolyl borate and
 tetradentate phenolate-based ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00604B
_journal_year                    2023
_chemical_formula_moiety
'2(C35 H31 B Cu Fe N12 O), 2(Cl O4), 2(C3 H7 N O), 4[C3H7NO]'
_chemical_formula_sum            'C88 H104 B2 Cl2 Cu2 Fe2 N30 O16'
_chemical_formula_weight         2169.31
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-02-24
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-25 deposited with the CCDC.	2023-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                95.765(4)
_cell_angle_beta                 105.730(4)
_cell_angle_gamma                108.664(3)
_cell_formula_units_Z            1
_cell_length_a                   12.1562(14)
_cell_length_b                   14.2336(16)
_cell_length_c                   15.5600(18)
_cell_measurement_reflns_used    9386
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.417
_cell_measurement_theta_min      2.710
_cell_volume                     2402.9(5)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'SADABS-20/2 (Bruker,2016/2)'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0584
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            52360
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.417
_diffrn_reflns_theta_min         2.710
_exptl_absorpt_coefficient_mu    0.870
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.901
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'metallic dark brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       prism
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       0.0019(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         12004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0637
_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^)+(0.0113P)^2^+10.3030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1319
_refine_ls_wR_factor_ref         0.1409
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9386
_reflns_number_total             12004
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00604b2.cif
_cod_data_source_block           9febf_0m
_cod_database_code               7712881
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.845
_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:
 C18(H18A,H18B), C26(H26A,H26B), C19(H19A,H19B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C12(H12), C4(H4), C9(H9), C11(H11), C16(H16), C13(H13), C15(H15),
 C7(H7), C24(H24), C28(H28), C8(H8), C34(H34), C36(H36), C5(H5), C21(H21),
 C29(H29), C6(H6), C14(H14), C23(H23), C22(H22), C31(H31), C33(H33), C32(H32)
2.d Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C37(H37A,H37B,H37C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 154 electrons were 
found in a volume of 515\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
4[C3H7NO] per Unit Cell 
which account for 160 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              53835
_shelx_hkl_checksum              62336
_shelx_fab_checksum              15563
_olex2_submission_special_instructions 'No special instructions were received'