Diiron Oxo Reactivity in a Weak-Field Environment
Betley, Theodore; Johnson, Elizabeth J.; Kleinlein, Claudia; Musgrave, Rebecca A.; Chemical Science  (2019) –; doi:10.1039/C9SC00605B

data_1551006
_publ_section_title
;
 Diiron Oxo Reactivity in a Weak-Field Environment
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC00605B
_journal_year                    2019
_chemical_formula_sum            'C68.09 H91.24 Fe2 N4 O4.53'
_chemical_formula_weight         1149.93
_chemical_name_systematic        tBudmxFe2OHMesthf
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-06-07 deposited with the CCDC.    2019-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.397(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.416(3)
_cell_length_b                   15.512(2)
_cell_length_c                   24.559(4)
_cell_measurement_reflns_used    525
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.33
_cell_measurement_theta_min      2.44
_cell_volume                     6364.9(17)
_computing_cell_refinement       'SAINT 8.34C (Bruker-AXS, 2014)'
_computing_data_collection       'APEX3 v2015.5-2 (Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT 8.34C (Bruker-AXS, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2015)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type
;
Bruker D8 goniometer with CMOS area detector  
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'I\mS microfocus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1905
_diffrn_reflns_av_unetI/netI     0.2249
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            33872
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.202
_diffrn_reflns_theta_max         25.202
_diffrn_reflns_theta_min         1.280
_exptl_absorpt_coefficient_mu    0.506
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6496
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow-brown
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_description       plate
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     728
_refine_ls_number_reflns         11345
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.2133
_refine_ls_R_factor_gt           0.0836
_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^)+(0.0720P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1477
_refine_ls_wR_factor_ref         0.1915
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4989
_reflns_number_total             11345
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00605b2.cif
_cod_data_source_block           tBudmxFe2OHMesthf
_cod_original_cell_volume        6364.8(16)
_cod_database_code               1551006
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.946
_shelx_estimated_absorpt_t_max   0.990
_shelx_res_checksum              30450