Catalytic Perchlorate Reduction Using Iron: Mechanistic Insights and Improved Catalyst Turnover
Drummond, Michael J.; Miller, Tabitha J.; Ford, Courtney L.; Fout, Alison R.; ACS Catalysis  (2020) 3175–3182; doi:10.1021/acscatal.9b05029

data_4517431
_publ_contact_author
; 
Danielle L. Gray 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_section_title
;
 Catalytic Perchlorate Reduction Using Iron: Mechanistic Insights and
 Improved Catalyst Turnover
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              3175
_journal_page_last               3182
_journal_paper_doi               10.1021/acscatal.9b05029
_journal_year                    2020
_chemical_formula_moiety         'C36 H51 Cl N7 Zn, C F3 O3 S'
_chemical_formula_sum            'C37 H51 Cl F3 N7 O3 S Zn'
_chemical_formula_weight         831.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
; 
? 
;
_cell_angle_alpha                90
_cell_angle_beta                 95.7511(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4934(3)
_cell_length_b                   24.7612(6)
_cell_length_c                   13.0442(3)
_cell_measurement_reflns_used    12634
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.41
_cell_measurement_theta_min      2.27
_cell_volume                     4014.93(17)
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2014)'
_computing_data_collection       'APEX3 V2016.9-0 (Bruker, 2016)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2014/2, (Bruker, 2014) SADABS V2014/7 
(Krause et al., 2015) 
;
_computing_molecular_graphics
; 
SHELXTL v2014-7 (Bruker, 2014), CrystalMaker v2.7.7 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'
_computing_structure_refinement  'SHELXL-2014-7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2014-7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Bruker D8 Venture/Photon 100'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  dd53rs_sq
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            38886
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.420
_diffrn_reflns_theta_min         2.273
_exptl_absorpt_coefficient_mu    0.789
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/7 (Krause et al., 2015)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1744
_exptl_crystal_id                dd53rs_sq
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Paratone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (1 2 -1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.041
_platon_squeeze_details
;
The electron count from the "squeeze" model converged in good agreement with
the number of solvate molecules predicted by the complete refinement.  
Squeeze removed 19 electrons from each of two void spaces in the P1 cell;
these two void spaces are symmetry equivalents in the true space group. The
most likely solution is one in which each of these void spaces is occupied
by one or two water molecules.
;
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         7382
_refine_ls_number_restraints     895
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0245P)^2^+6.4276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5637
_reflns_number_total             7382
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b05029_si_001.cif
_cod_data_source_block           dd53rs_sq
_cod_depositor_comments          'Adding full bibliography for 4517431.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4517431
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.878
_shelx_estimated_absorpt_t_max   0.968
_shelx_res_checksum              95958
_shelx_hkl_checksum              44990
_shelx_fab_checksum              26832
_platon_squeeze_void_probe_radius 1.20