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_4117948
_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
'0.85(C38 H10 B2 F24 Fe N6 O4), 0.15(C38 H12 F20 Fe N6 O4), C H Cl3'
_chemical_formula_sum            'C39 H11.31 B1.69 Cl3 F23.4 Fe N6 O4'
_chemical_formula_weight         1252.87
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.956(2)
_cell_angle_beta                 96.719(3)
_cell_angle_gamma                94.164(3)
_cell_formula_units_Z            2
_cell_length_a                   9.0623(4)
_cell_length_b                   13.5860(6)
_cell_length_c                   18.7510(9)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.00
_cell_measurement_theta_min      2.23
_cell_volume                     2240.31(18)
_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 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       '\w scans; 19 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  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            123350
_diffrn_reflns_theta_full        34.86
_diffrn_reflns_theta_max         34.86
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.664
_exptl_absorpt_correction_T_max  0.8786
_exptl_absorpt_correction_T_min  0.8731
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_description       Block
_exptl_crystal_F_000             1231
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.062
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.168
_refine_ls_hydrogen_treatment    Riding
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     751
_refine_ls_number_reflns         18479
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.168
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0425
_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          0.0521
_refine_ls_wR_factor_ref         0.0528
_reflns_number_gt                13767
_reflns_number_total             18479
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja300534r_si_002_2.cif
_cod_data_source_block           mjr14
_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 'Geometric positions' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_formula_sum        'C39 H11.31 B1.69 Cl3 F23.40 Fe N6 O4'
_cod_database_code               4117948