Investigation of SCO property‒structural relationships in a family of mononuclear Fe(ii) complexes
Chen, Xiu-Qin; Cai, You-De; Ye, Yi-Shan; Tong, Ming-Liang; Bao, Xin; Inorganic Chemistry Frontiers 6 (2019) 2194–; doi:10.1039/C9QI00577C

data_4350056
_publ_section_title
;
 Investigation of SCO property--structural relationships in a family of
 mononuclear Fe(ii) complexes
;
_journal_issue                   8
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              2194
_journal_paper_doi               10.1039/C9QI00577C
_journal_volume                  6
_journal_year                    2019
_chemical_absolute_configuration unk
_chemical_formula_moiety         '2(C13 H13 Fe0.5 N3 Se)'
_chemical_formula_sum            'C26 H26 Fe N6 Se2'
_chemical_formula_weight         636.30
_space_group_crystal_system      orthorhombic
_space_group_IT_number           30
_space_group_name_Hall           'P 2 -2bc'
_space_group_name_H-M_alt        'P n c 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-05-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2019-05-17 deposited with the CCDC.	2019-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.954(2)
_cell_length_b                   15.8604(19)
_cell_length_c                   8.7328(9)
_cell_measurement_reflns_used    3673
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      24.012
_cell_measurement_theta_min      2.502
_cell_volume                     2625.2(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 1.000
_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  0.1308
_diffrn_reflns_av_unetI/netI     0.1076
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            26281
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.470
_diffrn_reflns_theta_min         1.074
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.374
_exptl_absorpt_correction_T_max  0.0932
_exptl_absorpt_correction_T_min  0.0601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1069 before and 0.0734 after correction.
The Ratio of minimum to maximum transmission is 0.6448.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.034
_refine_diff_density_max         1.097
_refine_diff_density_min         -1.604
_refine_diff_density_rms         0.153
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.06(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         5319
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.1449
_refine_ls_R_factor_gt           0.0847
_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^)+(0.0202P)^2^+30.7685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1618
_refine_ls_wR_factor_ref         0.1843
_reflns_Friedel_coverage         0.869
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                3514
_reflns_number_total             5319
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9qi00577c2.cif
_cod_data_source_block           b_CCDC1
_cod_database_code               4350056
_shelx_estimated_absorpt_t_max   0.894
_shelx_estimated_absorpt_t_min   0.614
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.94(4) 0.06(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid bond restraints
 C18, C17, C16, C15, C14, N4, C22, C21, C20, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C19 \\sim C18 \\sim C17 \\sim C16 \\sim C15 \\sim C14 \\sim C22 \\sim C21 \\sim
C20 \\sim N4: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C7) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
5. Others
 Fixed Sof: Se2A(0.75) Se2B(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C24(H24A,H24B), C23(H23A,H23B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C8(H8), C18(H18), C7(H7), C5(H5), C4(H4), C15(H15), C20(H20),
 C17(H17), C21(H21), C16(H16)
6.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C25(H25A,H25B,H25C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'