Hydrogen Generation Catalyzed by Fluorinated Diglyoxime-Iron Complexes at Low Overpotentials
Michael J. Rose; Harry B. Gray; Jay R. Winkler; Journal of the American Chemical Society 134 (2012) 8310–8313; doi:10.1021/ja300534r

data_4117947
_publ_contact_author_address
;
Division of Chemistry and Chemical Engineering,
California Institute of Technology,
1200 E California Blvd,
Pasdena, CA 91125
USA
;
_publ_contact_author_email       mrose@caltech.edu
_publ_contact_author_fax         '+1 626 459 2935'
_publ_contact_author_name        'Michael Rose'
_publ_contact_author_phone       '+1 626 395 2846'
_publ_section_title
;
 Hydrogen Generation Catalyzed by Fluorinated Diglyoxime-Iron Complexes at
 Low Overpotentials
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8310
_journal_page_last               8313
_journal_paper_doi               10.1021/ja300534r
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C38 H12 F20 Fe N6 O4'
_chemical_formula_sum            'C38 H12 F20 Fe N6 O4'
_chemical_formula_weight         1052.39
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.991(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.0084(3)
_cell_length_b                   21.0943(8)
_cell_length_c                   11.4508(4)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.34
_cell_measurement_theta_min      2.65
_cell_volume                     1898.92(12)
_computing_cell_refinement       'Bruker SAINT-Plus v7.66A'
_computing_data_collection       'Bruker APEX2 v2009.7-0'
_computing_data_reduction        'Bruker SAINT-Plus v7.66A'
_computing_molecular_graphics    'Bruker XP v5.1'
_computing_publication_material  'Bruker XCIF 2008'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       '\w scans; 10 settings'
_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  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            51438
_diffrn_reflns_theta_full        33.60
_diffrn_reflns_theta_max         33.60
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_T_max  0.9471
_exptl_absorpt_correction_T_min  0.8795
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Violet
_exptl_crystal_density_diffrn    1.841
_exptl_crystal_description       Fragment
_exptl_crystal_F_000             1040
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_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
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_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    Unrestrained
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     341
_refine_ls_number_reflns         6985
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.186
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0416
_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^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0527
_refine_ls_wR_factor_ref         0.0534
_reflns_number_gt                5423
_reflns_number_total             6985
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja300534r_si_002_1.cif
_cod_data_source_block           mjr12
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_secondary' value 'Difference Fourier map' was
changed to 'difmap'.

'_atom_sites_solution_hydrogens' value 'Difference Fourier map' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               4117947