High-spin enforcement in first-row metal complexes of a constrained polyaromatic ligand: synthesis, structure, and properties
Chen, Lizhu; Dulaney, Hunter A.; Wilkins, Branford O.; Farmer, Sarah; Zhang, Yanbing; Fronczek, Frank R.; Jurss, Jonah W.; New Journal of Chemistry 42 (2018) 18667–; doi:10.1039/C8NJ02072H

data_7057837
_publ_section_title
;
 High-spin enforcement in first-row metal complexes of a constrained
 polyaromatic ligand: synthesis, structure, and properties
;
_journal_issue                   23
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18667
_journal_paper_doi               10.1039/C8NJ02072H
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety
'C35 H25 F3 Fe N5 O3 S, C F3 O3 S, 0.5(C4 H10 O)'
_chemical_formula_sum            'C38 H30 F6 Fe N5 O6.5 S2'
_chemical_formula_weight         894.64
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-10-12 deposited with the CCDC.
2018-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                86.1230(10)
_cell_angle_beta                 84.0350(10)
_cell_angle_gamma                81.0590(10)
_cell_formula_units_Z            2
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_cell_length_b                   13.9385(3)
_cell_length_c                   15.1654(3)
_cell_measurement_reflns_used    9758
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.51
_cell_volume                     1905.83(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_unetI/netI     0.0117
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            49150
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.355
_diffrn_reflns_theta_min         1.352
_exptl_absorpt_coefficient_mu    0.591
_exptl_absorpt_correction_T_max  0.9011
_exptl_absorpt_correction_T_min  0.8761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_description       block
_exptl_crystal_F_000             914
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         6873
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0270
_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^)+(0.0425P)^2^+1.6261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0745
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6460
_reflns_number_total             6873
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj02072h2.cif
_cod_data_source_block           5Fe
_cod_depositor_comments
'Adding full bibliography for 7057834--7057838.cif.'
_cod_original_formula_sum        'C38 H30 F6 Fe N5 O6.50 S2'
_cod_database_code               7057837
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.876
_shelx_estimated_absorpt_t_max   0.901
_shelx_res_checksum              94479