Low-spin [MII(L)2] and [MIII(L)2]+ (M = Fe and Co) complexes of tridentate azo-containing pyridine/pyrazine amide ligands: structures, properties and redox potential correlations
Sengupta, Arunava; Rajput, Amit; Barman, Suman K.; Mukherjee, Rabi; Dalton Trans.  (2017) –; doi:10.1039/C7DT01577A

data_7043848
_publ_section_title
;
 Low-spin [MII(L)2] and [MIII(L)2]+ (M = Fe and Co) complexes of
 tridentate azo-containing pyridine/pyrazine amide ligands: structures,
 properties and redox potential correlations
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01577A
_journal_year                    2017
_chemical_formula_moiety         'C36 H26 Fe N8 O2, 0.5(B2 F8)'
_chemical_formula_sum            'C36 H26 B F4 Fe N8 O2'
_chemical_formula_weight         745.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-10
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.05.22 svn.r3414 for OlexSys, GUI svn.r5347)
;
_audit_update_record
;
2017-07-12 deposited with the CCDC.
2017-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.882(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.714(2)
_cell_length_b                   24.385(2)
_cell_length_c                   11.8024(13)
_cell_measurement_reflns_used    2235
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      2.54
_cell_volume                     3809.9(7)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0941
_diffrn_reflns_av_unetI/netI     0.0791
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19603
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.023
_diffrn_reflns_theta_max         25.023
_diffrn_reflns_theta_min         2.041
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.457
_exptl_absorpt_correction_T_max  0.778
_exptl_absorpt_correction_T_min  0.085
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0678 before and 0.0430 after correction.
The Ratio of minimum to maximum transmission is 0.2956.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       block
_exptl_crystal_F_000             1524
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.740
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         3443
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1345
_refine_ls_R_factor_gt           0.0927
_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^)+(0.1660P)^2^+11.6420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2483
_refine_ls_wR_factor_ref         0.2778
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2235
_reflns_number_total             3443
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01577a2.cif
_cod_data_source_block           19juna_a_complex5
_cod_original_cell_volume        3810.0(8)
_cod_database_code               7043848
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 N3, C12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N4, C13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Fixed U11: F3(0.119231) F2(0.198794) F1(0.175955) B1(0.071281)
 Fixed U12: F3(0) F2(0) F1(-0.053432) B1(0)
 Fixed U13: F3(0.020081) F2(0.025178) F1(-0.012493) B1(0.016908)
 Fixed U22: F3(0.07111) F2(0.20152) F1(0.2582) B1(0.05399)
 Fixed U23: F3(0) F2(0) F1(0.01114) B1(0)
 Fixed U33: F3(0.28027) F2(0.19412) F1(0.19935) B1(0.14842)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C14(H14), C15(H15), C8(H8), C16(H16), C9(H9), C11(H11), C10(H10),
 C17(H17), C2(H2), C18(H18), C4(H4), C3(H3)
;
_shelx_res_checksum              43399
_shelx_fab_checksum              11081
_olex2_submission_special_instructions 'No special instructions were received'