Isolation and Characterization of a Dihydroxo-Bridged Iron(III,III)(μ-OH)2 Diamond Core Derived from Dioxygen
Michael K. Coggins; Santiago Toledo; Julie A. Kovacs; Inorganic Chemistry 52 (2013) 13325–13331; doi:10.1021/ic4010906

data_4336794
_publ_contact_author_address
;
Department of Chemistry, BOX 351700
University of Washington
Seattle, WA 98195
USA
;
_publ_contact_author_email       wernerka@u.washington.edu
_publ_contact_author_name        'Werner Kaminsky'
_publ_section_title
;
 Isolation and Characterization of a Dihydroxo-Bridged
 Iron(III,III)(\m-OH)2 Diamond Core Derived from Dioxygen
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13325
_journal_page_last               13331
_journal_paper_doi               10.1021/ic4010906
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C21 H29 Fe N4 O, F6 P'
_chemical_formula_sum            'C21 H29 F6 Fe N4 O P'
_chemical_formula_weight         553.40
_chemical_name_common            Santiago11
_chemical_name_systematic        Santiago11
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.9090(11)
_cell_length_b                   17.1316(12)
_cell_length_c                   17.6610(13)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    130(2)
_cell_volume                     4813.4(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'maXus, Zortep'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w 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  0.0825
_diffrn_reflns_av_sigmaI/netI    0.1622
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9203
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  0.9694
_exptl_absorpt_correction_T_min  0.9619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL2000
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_description       cut-block
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         4886
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.1772
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1548
_reflns_number_gt                2066
_reflns_number_total             4886
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4010906_si_003.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        4813.3(6)
_cod_original_sg_symbol_Hall     -p_2ac_2ab
_cod_database_code               4336794