An Iron-Based Dehydration Catalyst for Selective Formation of Styrene
Nachtigall, Olaf; VanderWeide, Andrew I.; Brennessel, William W.; Jones, William D.; ACS Catalysis  (2021) 10885–10891; doi:10.1021/acscatal.1c03037

data_4518959
_publ_section_title
;
 An Iron-Based Dehydration Catalyst for Selective Formation of Styrene
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              10885
_journal_page_last               10891
_journal_paper_doi               10.1021/acscatal.1c03037
_journal_year                    2021
_chemical_formula_moiety         'C18 H17 F6 Fe N3 O9 S2'
_chemical_formula_sum            'C18 H17 F6 Fe N3 O9 S2'
_chemical_formula_weight         653.32
_chemical_name_common            jonon95
_chemical_name_systematic        (FOX)Fe(OTf)2
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-11-19
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.8240(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.99030(10)
_cell_length_b                   15.5335(2)
_cell_length_c                   14.0576(2)
_cell_measurement_reflns_used    27130
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      77.5570
_cell_measurement_theta_min      4.2690
_cell_volume                     2364.69(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -49.00  22.00   0.50    0.05    --  -49.75  49.00  64.00  142
  2  \w    -49.00 -12.00   0.50    0.16    --  -84.25  49.00  64.00   74
  3  \w    -42.00 -12.00   0.50    0.16    --  -84.25  45.00-120.00   60
  4  \w   -121.00 -39.00   0.50    0.05    --  -49.75 -49.00 -82.00  164
  5  \w    -21.00  60.00   0.50    0.05    --   49.75 -49.00 -82.00  162
  6  \w     34.00  61.00   0.50    0.16    --  105.75 -49.00 -82.00   54
  7  \w     34.00  87.00   0.50    0.16    --  105.75 -61.00-120.00  106
  8  \w     98.00 164.00   0.50    0.16    --  105.75  15.00 -90.00  132
  9  \w     98.00 178.00   0.50    0.16    --  105.75  30.00   0.00  160
 10  \w     96.00 178.00   0.50    0.16    --  105.75  49.00  64.00  164
 11  \w     97.00 178.00   0.50    0.16    --  105.75  45.00 -60.00  162
 12  \w     98.00 164.00   0.50    0.16    --  105.75  15.00-180.00  132
 13  \w     92.00 178.00   0.50    0.16    --  105.75  61.00-180.00  172
 14  \w     92.00 178.00   0.50    0.16    --  105.75 125.00 -90.00  172
 15  \w     98.00 164.00   0.50    0.16    --  105.75  15.00   0.00  132
 16  \w     92.00 178.00   0.50    0.16    --  105.75 125.00 -30.00  172
 17  \w     40.00 121.00   0.50    0.05    --   49.75  49.00  64.00  162
 18  \w     34.00  87.00   0.50    0.16    --  105.75 -61.00  60.00  106
 19  \w     34.00  87.00   0.50    0.16    --  105.75 -61.00 150.00  106
 20  \w     34.00  87.00   0.50    0.16    --  105.75 -61.00  90.00  106
 21  \w     34.00  87.00   0.50    0.16    --  105.75 -61.00   0.00  106
 22  \w     34.00  87.00   0.50    0.16    --  105.75 -61.00 -60.00  106
 23  \w     34.00  87.00   0.50    0.16    --  105.75 -61.00-150.00  106
 24  \w     34.00  87.00   0.50    0.16    --  105.75 -61.00-180.00  106
 25  \w     34.00  87.00   0.50    0.16    --  105.75 -61.00 -30.00  106
 26  \w     29.00 121.00   0.50    0.05    --   49.75  77.00-150.00  184
 27  \w     29.00 121.00   0.50    0.05    --   49.75  77.00 -90.00  184
 28  \w     29.00  82.00   0.50    0.05    --   49.75  77.00-180.00  106
 29  \w     29.00 121.00   0.50    0.05    --   49.75  77.00 120.00  184
 30  \w   -121.00 -70.00   0.50    0.05    --  -49.75-125.00  60.00  102
 31  \w   -121.00 -70.00   0.50    0.05    --  -49.75-125.00  30.00  102
 32  \w   -121.00 -37.00   0.50    0.05    --  -49.75 -57.00   0.00  168
 33  \w   -121.00 -70.00   0.50    0.05    --  -49.75-125.00-150.00  102
 34  \w   -156.00 -74.00   0.50    0.16    --  -84.25 -49.00 -82.00  164
 35  \w   -121.00 -29.00   0.50    0.05    --  -49.75 -77.00  90.00  184
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0570046000
_diffrn_orient_matrix_UB_12      -0.0597009000
_diffrn_orient_matrix_UB_13      -0.0832406000
_diffrn_orient_matrix_UB_21      -0.1272724000
_diffrn_orient_matrix_UB_22      0.0095589000
_diffrn_orient_matrix_UB_23      0.0307500000
_diffrn_orient_matrix_UB_31      -0.0280165000
_diffrn_orient_matrix_UB_32      0.0786870000
_diffrn_orient_matrix_UB_33      -0.0669876000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            40193
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         79.787
_diffrn_reflns_theta_min         4.277
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.749
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.221
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.142
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         4997
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+1.8932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0812
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4757
_reflns_number_total             4997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c03037_si_002.cif
_cod_data_source_block           A
_cod_database_code               4518959
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.406
_shelx_estimated_absorpt_t_min   0.279
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C4(H4), C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B)
2.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15), C16(H16)
;
_shelx_res_checksum              72801
_olex2_submission_original_sample_id jonon95
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.424
_oxdiff_exptl_absorpt_empirical_full_min 0.822