Water-Soluble Fe(II)-H2O Complex with a Weak O-H Bond Transfers a Hydrogen Atom via an Observable Monomeric Fe(III)-OH.
Brines, Lisa M.; Coggins, Michael K.; Poon, Penny Chaau Yan; Toledo, Santiago; Kaminsky, Werner; Kirk, Martin L.; Kovacs, Julie A.; Journal of the American Chemical Society 137 (2015) 2253–2264; doi:10.1021/ja5068405

data_4123368
_publ_section_title
;
 Water-Soluble Fe(II)-H2O Complex with a Weak O-H Bond Transfers a
 Hydrogen Atom via an Observable Monomeric Fe(III)-OH.
;
_journal_issue                   6
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2253
_journal_page_last               2264
_journal_paper_doi               10.1021/ja5068405
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety
'2(C22 H51 Fe2 N8 O3), C4 H10 O, 6(C F3 O3 S)'
_chemical_formula_sum            'C54 H112 F18 Fe4 N16 O25 S6'
_chemical_formula_weight         2143.42
_chemical_name_common            brines08_b
_chemical_name_systematic        brines08_b
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 111.1170(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   20.5640(5)
_cell_length_b                   13.0420(4)
_cell_length_c                   18.4360(7)
_cell_measurement_reflns_used    798
_cell_measurement_temperature    130(2)
_cell_volume                     4612.4(3)
_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    SIR97
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.901
_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  0.0919
_diffrn_reflns_av_sigmaI/netI    0.1891
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17909
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_T_max  0.8888
_exptl_absorpt_correction_T_min  0.6626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL2000
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2220
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.277
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         10375
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.2041
_refine_ls_R_factor_gt           0.0655
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1760
_reflns_number_gt                4065
_reflns_number_total             10375
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5068405_si_003.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 4123366--4123368.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4123368