Photoinduced O<sub>2</sub>-Dependent Stepwise Oxidative Deglycination of a Nonheme Iron(III) Complex.
Wegeberg, Christina; Fernández-Alvarez, Víctor M; de Aguirre, Adiran; Frandsen, Cathrine; Browne, Wesley R.; Maseras, Feliu; McKenzie, Christine J.; Journal of the American Chemical Society 140 (2018) 14150–14160; doi:10.1021/jacs.8b07455

data_4132933
_publ_section_title
;
 Photoinduced O<sub>2</sub>-Dependent Stepwise Oxidative Deglycination of
 a Nonheme Iron(III) Complex.
;
_journal_issue                   43
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14150
_journal_page_last               14160
_journal_paper_doi               10.1021/jacs.8b07455
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C42 H45 Fe N10 O2 Zn, 3(Cl O4), 1.5(H2O)'
_chemical_formula_sum            'C42 H45 Cl3 Fe N10 O15.5 Zn'
_chemical_formula_weight         1165.44
_chemical_name_common            '[Fe(SBPy3)Zn(tpena)](ClO4)6(H2O)3'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.3863(3)
_cell_length_b                   17.7438(4)
_cell_length_c                   40.7345(13)
_cell_measurement_reflns_used    12889
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.4030
_cell_measurement_theta_min      4.0980
_cell_volume                     9675.4(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.12b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.12b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.12b (Rigaku OD, 2015)'
_computing_molecular_graphics
'Mercury 3.9 (Macrae at al., 2008) and POV-RAY (Cason, 2004)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXL-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.2923
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0717
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            33496
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.948
_diffrn_reflns_theta_min         3.303
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    5.230
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.286
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.39.12b (Rigaku Oxford Diffraction, 2015) 
Numerical absorption correction based on gaussian integration over 
   a multifaceted crystal model 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            'clear dark purple'
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_description       needle
_exptl_crystal_F_000             4784
_exptl_crystal_size_max          0.524
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.054
_refine_diff_density_max         1.421
_refine_diff_density_min         -1.025
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.431(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1307
_refine_ls_number_reflns         18082
_refine_ls_number_restraints     1422
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0765
_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^)+(0.0738P)^2^+45.8641P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1840
_refine_ls_wR_factor_ref         0.1885
_reflns_Friedel_coverage         0.835
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                16800
_reflns_number_total             18082
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b07455_si_002.cif
_cod_data_source_block           CW_a_a
_cod_depositor_comments
;

2020-05-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C84 H90 Cl6 Fe2 N20 O31 Zn2'
_cod_original_formula_weight         2330.89
_cod_original_formula_moiety         '(C42 H45 Fe N10 O2 Zn)2, (Cl O4)6, (H2O)3'
_cod_original_formula_units_Z            4
_cod_database_code               4132933
_shelx_estimated_absorpt_t_min   0.170
_shelx_estimated_absorpt_t_max   0.765
_shelxl_version_number           2014/6
_shelx_res_checksum              33783
_shelx_hkl_checksum              91817