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_4518960
_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         'C23 H29 F3 Fe N3 O7 S, C F3 O3 S, C6 H12 O'
_chemical_formula_sum            'C30 H41 F6 Fe N3 O11 S2'
_chemical_formula_weight         853.63
_chemical_name_common            jonon94
_chemical_name_systematic        '[(FOX)Fe(CyOH)(OTf)][OTf-CyOH]'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                77.548(2)
_cell_angle_beta                 80.246(2)
_cell_angle_gamma                80.970(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0940(2)
_cell_length_b                   13.5688(3)
_cell_length_c                   14.2285(2)
_cell_measurement_reflns_used    29439
_cell_measurement_temperature    100.00(13)
_cell_measurement_theta_max      77.2340
_cell_measurement_theta_min      3.2270
_cell_volume                     1860.69(6)
_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      100.00(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.973
_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    -21.00  75.00   0.50    0.17    --   49.75 -87.00-111.00  192
  2  \w     34.00 131.00   0.50    0.68    --  105.75 -87.00-111.00  194
  3  \w     98.00 164.00   0.50    0.68    --  105.75  15.00 -60.00  132
  4  \w     98.00 178.00   0.50    0.68    --  105.75  87.00   6.00  160
  5  \w     98.00 164.00   0.50    0.68    --  105.75  15.00   0.00  132
  6  \w     98.00 178.00   0.50    0.68    --  105.75  30.00  30.00  160
  7  \w     98.00 164.00   0.50    0.68    --  105.75  15.00  90.00  132
  8  \w     92.00 178.00   0.50    0.68    --  105.75  61.00 -30.00  172
  9  \w     98.00 178.00   0.50    0.68    --  105.75  30.00-180.00  160
 10  \w     92.00 178.00   0.50    0.68    --  105.75 125.00-120.00  172
 11  \w     92.00 178.00   0.50    0.68    --  105.75  61.00  60.00  172
 12  \w     83.00 178.00   0.50    0.68    --  105.75  81.00 -84.84  190
 13  \w     92.00 178.00   0.50    0.68    --  105.75 125.00-150.00  172
 14  \w     34.00  87.00   0.50    0.68    --  105.75 -61.00-120.00  106
 15  \w     34.00 113.00   0.50    0.68    --  105.75-118.00-156.77  158
 16  \w     34.00 109.00   0.50    0.68    --  105.75 -94.00   0.00  150
 17  \w     34.00 116.00   0.50    0.68    --  105.75-125.00 150.00  164
 18  \w     34.00  87.00   0.50    0.68    --  105.75 -61.00 150.00  106
 19  \w     34.00 109.00   0.50    0.68    --  105.75 -94.00  60.00  150
 20  \w     34.00 111.00   0.50    0.68    --  105.75-108.00 -28.82  154
 21  \w     34.00 109.00   0.50    0.68    --  105.75 -94.00-180.00  150
 22  \w     34.00 127.00   0.50    0.68    --  105.75 -77.00-150.00  186
 23  \w     34.00 109.00   0.50    0.68    --  105.75 -94.00-120.00  150
 24  \w     34.00 109.00   0.50    0.68    --  105.75 -94.00-150.00  150
 25  \w     34.00  87.00   0.50    0.68    --  105.75 -61.00   0.00  106
 26  \w     34.00 109.00   0.50    0.68    --  105.75 -94.00  30.00  150
 27  \w     34.00 109.00   0.50    0.68    --  105.75 -94.00 -30.00  150
 28  \w     34.00  87.00   0.50    0.68    --  105.75 -61.00 -60.00  106
 29  \w     34.00  87.00   0.50    0.68    --  105.75 -61.00  30.00  106
 30  \w     34.00 116.00   0.50    0.68    --  105.75-125.00  90.00  164
 31  \w     34.00 109.00   0.50    0.68    --  105.75 -94.00 150.00  150
 32  \w    -23.00   5.00   0.50    0.17    --   49.75 -19.00 120.00   56
 33  \w    -23.00   5.00   0.50    0.17    --   49.75 -19.00   0.00   56
 34  \w    -23.00   5.00   0.50    0.17    --   49.75 -19.00 -60.00   56
 35  \w    -23.00   5.00   0.50    0.17    --   49.75 -19.00 -90.00   56
 36  \w    -23.00   5.00   0.50    0.17    --   49.75 -19.00 -30.00   56
 37  \w     29.00  90.00   0.50    0.17    --   49.75  77.00 -30.00  122
 38  \w     29.00 121.00   0.50    0.17    --   49.75  77.00-120.00  184
 39  \w    -30.00  22.00   0.50    0.17    --  -49.75  38.00 -90.00  104
 40  \w    -42.00 -12.00   0.50    0.68    --  -84.25  45.00-150.00   60
 41  \w    -75.00  22.00   0.50    0.17    --  -49.75  87.00   6.00  194
 42  \w    -42.00 -12.00   0.50    0.68    --  -84.25  45.00   0.00   60
 43  \w   -109.00 -12.00   0.50    0.68    --  -84.25  87.00   6.00  194
 44  \w   -121.00 -37.00   0.50    0.17    --  -49.75 -57.00 120.00  168
 45  \w   -121.00 -70.00   0.50    0.17    --  -49.75-125.00   0.00  102
 46  \w   -121.00 -70.00   0.50    0.17    --  -49.75-125.00  30.00  102
 47  \w   -121.00 -70.00   0.50    0.17    --  -49.75-125.00 120.00  102
 48  \w   -156.00 -76.00   0.50    0.68    --  -84.25 -87.00-111.00  160
;
_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      -0.0741155000
_diffrn_orient_matrix_UB_12      -0.0886981000
_diffrn_orient_matrix_UB_13      0.0609790000
_diffrn_orient_matrix_UB_21      -0.0893366000
_diffrn_orient_matrix_UB_22      0.0106005000
_diffrn_orient_matrix_UB_23      -0.0802029000
_diffrn_orient_matrix_UB_31      0.1043497000
_diffrn_orient_matrix_UB_32      -0.0758595000
_diffrn_orient_matrix_UB_33      -0.0489038000
_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  0.0710
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            46235
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         79.127
_diffrn_reflns_theta_min         3.213
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.107
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58008
_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    1.524
_exptl_crystal_description       block
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.237
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.0159
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         7836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0865P)^2^+1.2450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1472
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7318
_reflns_number_total             7836
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c03037_si_002.cif
_cod_data_source_block           B
_cod_original_cell_volume        1860.70(6)
_cod_database_code               4518960
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.923
_shelx_estimated_absorpt_t_min   0.377
_reflns_odcompleteness_completeness 99.86
_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), C18(H18), C25(H25)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C19(H19A,H19B), C20(H20A,H20B),
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C26(H26A,H26B), C27(H27A,H27B),
  C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B)
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              30239
_olex2_submission_original_sample_id jonon94
_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 2.577
_oxdiff_exptl_absorpt_empirical_full_min 0.490