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_7712880
_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
'C34 H32 B Cl Fe Mn N13 O, 2(C3 H7 N O), 1[C3H7NO]'
_chemical_formula_sum            'C43 H53 B Cl Fe Mn N16 O4'
_chemical_formula_weight         1015.06
_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             2023-02-15
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-15 deposited with the CCDC.	2023-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                104.669(2)
_cell_angle_beta                 93.059(2)
_cell_angle_gamma                101.198(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3138(6)
_cell_length_b                   16.1466(11)
_cell_length_c                   16.5173(10)
_cell_measurement_reflns_used    4790
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.238
_cell_measurement_theta_min      2.633
_cell_volume                     2343.5(3)
_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 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_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  0.1684
_diffrn_reflns_av_unetI/netI     0.1857
_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       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33873
_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         28.238
_diffrn_reflns_theta_min         2.633
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4210
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'NOT MEASURED'
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       0.0041(7)
_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   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         11551
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1448
_refine_ls_R_factor_gt           0.0748
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0621P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1563
_refine_ls_wR_factor_ref         0.1925
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6419
_reflns_number_total             11551
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00604b2.cif
_cod_data_source_block           3deca_0m
_cod_database_code               7712880
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.746
_shelx_estimated_absorpt_t_min   0.421
_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, All O(H) groups
2. Restrained distances
 O1-H1A
 0.85 with sigma of 0.01
 Mn1-H1A
 3.018513 with sigma of 0.02
 C34-H1A
 1.848363 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 B1(H1)
3.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C28(H28A,H28B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C16(H16), C12(H12), C5(H5), C17(H17), C10(H10), C14(H14), C27(H27),
 C24(H24), C6(H6), C15(H15), C11(H11), C26(H26), C25(H25), C7(H7), C32(H32),
 C33(H33), C9(H9), C8(H8), C30(H30), C31(H31), C35(H35), C38(H38)
3.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C36(H36A,H36B,H36C), C40(H40A,H40B,H40C), C39(H39A,H39B,
 H39C), C37(H37A,H37B,H37C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 76 electrons were found in a volume of 284\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 1[C3H7NO] per Asymmetric Unit 
which account for 80 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              93021
_shelx_hkl_checksum              26293
_shelx_fab_checksum              39497
_olex2_submission_special_instructions 'No special instructions were received'