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_4003872
_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         '0.02(O120 Si60), 0.09(F), 0.1(C8 H15 N2)'
_chemical_formula_sum            'C0.8 H1.5 F0.09 N0.2 O2 Si'
_chemical_formula_weight         75.69
_space_group_crystal_system      hexagonal
_space_group_IT_number           178
_space_group_name_Hall           'P 61 2 (0 0 5)'
_space_group_name_H-M_alt        'P 61 2 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-05-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506),
 SHELXL-2018/3, and manual edit
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            60
_cell_length_a                   11.881(2)
_cell_length_b                   11.881(2)
_cell_length_c                   29.696(5)
_cell_measurement_reflns_used    8213
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      77.5
_cell_measurement_theta_min      4.3
_cell_volume                     3630.2(11)
_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-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2013)'
_diffrn_ambient_temperature      298.15
_diffrn_detector                 'CPAD Area Detector'
_diffrn_detector_area_resol_mean 7.69
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.943
_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  0.0646
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            12242
_diffrn_reflns_point_group_measured_fraction_full 0.947
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         77.482
_diffrn_reflns_theta_min         4.297
_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    6.164
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7433
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1157 before and 0.0785 after correction.
The Ratio of minimum to maximum transmission is 0.7433.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.077
_exptl_crystal_description       prism
_exptl_crystal_F_000             2310
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details
;
 Flack x determined using 695 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         2342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0548P)^2^+19.2206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1391
_reflns_Friedel_coverage         0.551
_reflns_Friedel_fraction_full    0.910
_reflns_Friedel_fraction_max     0.853
_reflns_number_gt                2146
_reflns_number_total             2342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c04573_si_003.cif
_cod_data_source_block           v19152
_cod_original_cell_volume        3630.5(14)
_cod_original_sg_symbol_Hall     'P 61 2 (0 0 -1)'
_cod_original_formula_sum        'C0.80 H1.50 F0.09 N0.20 O2 Si'
_cod_database_code               4003872
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.791
_shelx_estimated_absorpt_t_min   0.607
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{N1, C3A}
{C1, N2A}
{C2, C2A}
{C4, C8A}
{C6, C7A}
3. Uiso/Uaniso restraints and constraints
Uanis(N1) = Uanis(C3A)
Uanis(C1) = Uanis(N2A)
Uanis(C4) = Uanis(C8A)
Uanis(C6) = Uanis(C7A)
Uanis(C2) = Uanis(C2A)
4. Others
 Fixed Sof: N1(0.5) C1(0.5) C2(0.25) H2(0.25) C4(0.5) H4A(0.5) H4B(0.5)
 C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5) C6(0.5) H6A(0.5) H6B(0.5) H6C(0.5) N2A(0.5)
 C2A(0.25) H2B(0.25) C3A(0.5) C7A(0.5) H7A(0.5) H7B(0.5) H7C(0.5) C8A(0.5)
 H8A(0.5) H8B(0.5) H8C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C2A(H2B)
5.c Idealised Me refined with riding coordinates:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7A(H7A,H7B,H7C), C8A(H8A,H8B,H8C)
;
_shelx_res_checksum              76988
_shelx_hkl_checksum              8132
_olex2_submission_special_instructions 'No special instructions were received'