Molecular Structure of Copper and μ-Oxodiiron Octafluorocorrole Derivatives: Insights into Ligand Noninnocence
Thomas, Kolle E.; Settineri, Nicholas S.; Teat, Simon J.; Steene, Erik; Ghosh, Abhik; ACS Omega  (2020) –; doi:10.1021/acsomega.0c01035

data_4517602
_publ_section_title
;
 Molecular Structure of Copper and \m-Oxodiiron Octafluorocorrole
 Derivatives: Insights into Ligand Noninnocence
;
_journal_name_full               'ACS Omega'
_journal_paper_doi               10.1021/acsomega.0c01035
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C74 H30 F16 Fe2 N8 O'
_chemical_formula_sum            'C74 H30 F16 Fe2 N8 O'
_chemical_formula_weight         1462.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 98.773(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.065(3)
_cell_length_b                   21.913(3)
_cell_length_c                   16.255(3)
_cell_measurement_reflns_used    9751
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.62
_cell_measurement_theta_min      2.84
_cell_volume                     7063.5(19)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker D8 PHOTON-II CMOS'
_diffrn_measurement_method       '\w/q shutterless scans'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            51140
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        22.500
_diffrn_reflns_theta_max         22.654
_diffrn_reflns_theta_min         2.106
_diffrn_source                   'Advanced Light Source beamline 12.2.1'
_exptl_absorpt_coefficient_mu    0.533
_exptl_absorpt_correction_T_max  0.7448
_exptl_absorpt_correction_T_min  0.5439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       needle
_exptl_crystal_F_000             2936
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.854
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         8592
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0669
_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^)+(0.1483P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1728
_refine_ls_wR_factor_ref         0.1774
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                7988
_reflns_number_total             8592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c01035_si_003.cif
_cod_data_source_block           F8FeTPC_O
_cod_original_cell_volume        7063.4(19)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4517602
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.939
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              38618
_shelx_hkl_checksum              568