Further Investigations of Racemic and Chiral Molecular Sieves of the STW Topology
Kang, Jong Hun; McCusker, Lynne B.; Deem, Michael W.; Baerlocher, Christian; Davis, Mark E.; Chemistry of Materials  (2021) –; doi:10.1021/acs.chemmater.0c04573

data_4003873
_publ_section_title
;
 Further Investigations of Racemic and Chiral Molecular Sieves of the STW
 Topology
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.0c04573
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         '10(O2 Si1), 0.89(F), C8 H15 N2'
_chemical_formula_sum            'C8 H15 F0.89 N2 O20 Si10'
_chemical_formula_weight         757.09
_space_group_crystal_system      hexagonal
_space_group_IT_number           179
_space_group_name_Hall           'P 65 2 (0 0 1)'
_space_group_name_H-M_alt        'P 65 2 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-02-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506),
 SHELXL-2017/1, and manual edit
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   11.9347(18)
_cell_length_b                   11.9347(18)
_cell_length_c                   29.530(4)
_cell_measurement_reflns_used    9820
_cell_measurement_temperature    298
_cell_measurement_theta_max      77.35
_cell_measurement_theta_min      4.28
_cell_volume                     3642.6(9)
_computing_cell_refinement       'SAINT V8.38A (Bruker-AXS, 2016)'
_computing_data_collection
'BIS V6.2.9/2018-03-16 & APEX3 v2018.7-2 (Bruker-AXS, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker-AXS, 2016)'
_computing_molecular_graphics    'DIAMOND 3 (Crystal Impact, 1999)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2013)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'CPAD Area Detector'
_diffrn_detector_area_resol_mean 7.69
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            16240
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         77.613
_diffrn_reflns_theta_min         4.277
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\mS HB'
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.144
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7296
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.0992 before and 0.0803 after correction. 
The Ratio of minimum to maximum transmission is 0.7296. 
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.071
_exptl_crystal_description       prism
_exptl_crystal_F_000             2310
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 810 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.07(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2443
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0252P)^2^+6.5765P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0807
_reflns_Friedel_coverage         0.598
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.931
_reflns_number_gt                2262
_reflns_number_total             2443
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c04573_si_002.cif
_cod_data_source_block           v19009
_cod_original_cell_volume        3642.6(12)
_cod_database_code               4003873
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.887
_shelx_estimated_absorpt_t_min   0.791
_refine_ls_abs_structure_hooft   0.05(2)
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Shared sites
{C1, N1}
3. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(N1)
4. Others
 Fixed Sof: C1(0.5) N1(0.5) H3A(0.5) H3B(0.5) H3C(0.5) H3D(0.5) H3E(0.5)
 H3F(0.5) H5A(0.5) H5B(0.5) H5C(0.5)
5.a Me refined with riding coordinates:
 C5(H5A,H5B,H5C)
5.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C3(H3D,H3E,H3F), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              83200
_shelx_hkl_checksum              10287
_olex2_submission_special_instructions 'No special instructions were received'