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_4518961
_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         'C16 H21 Fe N3 O5, 2(C F3 O3 S)'
_chemical_formula_sum            'C18 H21 F6 Fe N3 O11 S2'
_chemical_formula_weight         689.35
_chemical_name_common            jonon101
_chemical_name_systematic        '[(FOX)Fe(H2O)2][OTf]2'
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-11-11
_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                 100.509(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3968(2)
_cell_length_b                   9.43800(10)
_cell_length_c                   20.5184(3)
_cell_measurement_reflns_used    20479
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.7400
_cell_measurement_theta_min      3.3440
_cell_volume                     2550.81(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(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_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     33.00 121.00   0.50    0.20    --   49.87  69.00 129.00  176
  2  \w     89.00 178.00   0.50    0.80    --  105.75  69.00 129.00  178
  3  \w     98.00 164.00   0.50    0.80    --  105.75  15.00 150.00  132
  4  \w     98.00 164.00   0.50    0.80    --  105.75  15.00  90.00  132
  5  \w     98.00 164.00   0.50    0.80    --  105.75  15.00  60.00  132
  6  \w     92.00 178.00   0.50    0.80    --  105.75  61.00  60.00  172
  7  \w     97.00 178.00   0.50    0.80    --  105.75  45.00-120.00  162
  8  \w     98.00 164.00   0.50    0.80    --  105.75  15.00-150.00  132
  9  \w    -42.00 -12.00   0.50    0.80    --  -84.25  45.00 -90.00   60
 10  \w    -67.00  22.00   0.50    0.20    --  -49.87  69.00 129.00  178
 11  \w     34.00 116.00   0.50    0.80    --  105.75-125.00 150.00  164
 12  \w     34.00 116.00   0.50    0.80    --  105.75-125.00  30.00  164
 13  \w   -101.00 -12.00   0.50    0.80    --  -84.25  69.00 129.00  178
 14  \w   -121.00 -70.00   0.50    0.20    --  -49.87-125.00 -90.00  102
 15  \w   -121.00 -33.00   0.50    0.20    --  -49.87 -69.00  -3.00  176
 16  \w    -21.00  67.00   0.50    0.20    --   49.87 -69.00  -3.00  176
 17  \w    -22.00   5.00   0.50    0.20    --   49.87 -19.00-120.00   54
 18  \w    -22.00   5.00   0.50    0.20    --   49.87 -19.00-150.00   54
 19  \w    -22.00   5.00   0.50    0.20    --   49.87 -19.00   0.00   54
 20  \w     34.00  87.00   0.50    0.80    --  105.75 -61.00-120.00  106
 21  \w     34.00 127.00   0.50    0.80    --  105.75 -77.00-180.00  186
 22  \w     34.00  87.00   0.50    0.80    --  105.75 -61.00 -60.00  106
 23  \w     34.00  87.00   0.50    0.80    --  105.75 -61.00 -90.00  106
 24  \w     34.00 123.00   0.50    0.80    --  105.75 -69.00  -3.00  178
 25  \w     34.00  87.00   0.50    0.80    --  105.75 -61.00  30.00  106
 26  \w     34.00  87.00   0.50    0.80    --  105.75 -61.00 150.00  106
;
_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      -0.0696318000
_diffrn_orient_matrix_UB_12      0.0579817000
_diffrn_orient_matrix_UB_13      -0.0623790000
_diffrn_orient_matrix_UB_21      0.0799381000
_diffrn_orient_matrix_UB_22      0.1134556000
_diffrn_orient_matrix_UB_23      -0.0071843000
_diffrn_orient_matrix_UB_31      0.0493743000
_diffrn_orient_matrix_UB_32      -0.1020273000
_diffrn_orient_matrix_UB_33      -0.0434549000
_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  0.0449
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33019
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.699
_diffrn_reflns_theta_min         3.355
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.280
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56339
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.073
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         5380
_refine_ls_number_restraints     306
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0435P)^2^+1.4330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0825
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5089
_reflns_number_total             5380
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c03037_si_002.cif
_cod_data_source_block           C
_cod_database_code               4518961
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.619
_shelx_estimated_absorpt_t_min   0.318
_reflns_odcompleteness_completeness 100.00
_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. Restrained distances
 S2-C18 \\sim S2-C18'
 with sigma of 0.01
 S2-O9 \\sim S2-O10 \\sim S2-O11 \\sim S2-O9' \\sim S2-O10' \\sim S2-O11'
 with sigma of 0.01
 O9-O10 \\sim O10-O11 \\sim O11-O9 \\sim O9'-O10' \\sim O10'-O11' \\sim O11'-O9'
 with sigma of 0.02
 C18-F4 \\sim C18-F5 \\sim C18-F6 \\sim C18'-F4' \\sim C18'-F5' \\sim C18'-F6'
 with sigma of 0.01
 F4-F5 \\sim F5-F6 \\sim F6-F4 \\sim F4'-F5' \\sim F5'-F6' \\sim F6'-F4'
 with sigma of 0.02
 S1-C17 \\sim S1-C17'
 with sigma of 0.01
 C17-F1 \\sim C17-F2 \\sim C17-F3 \\sim C17'-F1' \\sim C17'-F2' \\sim C17'-F3'
 with sigma of 0.01
 F1-F2 \\sim F2-F3 \\sim F3-F1 \\sim F1'-F2' \\sim F2'-F3' \\sim F3'-F1'
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.2A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 1.2A
4. Rigid body (RIGU) restrains
 S2, F4, F5, F6, O9, O10, O11, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S2, F4', F5', F6', O9', O10', O11', C18'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1, F2, F3, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1', F2', F3', C17'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F4')=Sof(F5')=Sof(F6')=Sof(O9')=Sof(O10')=Sof(O11')=Sof(C18')=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=Sof(O9)=Sof(O10)=Sof(O11)=Sof(C18)=FVAR(1)
 Sof(F1')=Sof(F2')=Sof(F3')=Sof(C17')=1-FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(C17)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C4(H4), C6(H6)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5C,H5D)
6.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              94067
_olex2_submission_original_sample_id jonon101
_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 1.904
_oxdiff_exptl_absorpt_empirical_full_min 0.672