A fluoride-free siliceous STW-type zeolite synthesized using a designed organic structure-directing agent.
Jiao, Feng; Zhang, Jun; Cai, Xianshu; Li, Hao; Xu, Yanan; Zhao, Yue; Du, Hongbin; Chemical communications (Cambridge, England) 59 (2023) 1649–1652; doi:10.1039/d2cc05850b

data_7131208
_publ_section_title
;
 A fluoride-free siliceous STW-type zeolite synthesized using a designed
 organic structure-directing agent.
;
_journal_issue                   12
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1649
_journal_page_last               1652
_journal_paper_doi               10.1039/d2cc05850b
_journal_volume                  59
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'O20 Si10, C8 H15 N2, F'
_chemical_formula_sum            'C8 H15 F N2 O20 Si10'
_chemical_formula_weight         759.12
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-16
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-10-19 deposited with the CCDC.	2023-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   11.8995(9)
_cell_length_b                   11.8995(9)
_cell_length_c                   29.636(4)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    210
_cell_measurement_theta_max      56.82
_cell_measurement_theta_min      3.73
_cell_volume                     3634.2(6)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX4 V2022.1-1 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      210
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Metaljet PHOTON II'
_diffrn_measurement_method       '\w and \f shutterless scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_monochromator  'Helios Multi-layer Optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0953
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            18960
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         56.992
_diffrn_reflns_theta_min         3.732
_diffrn_source                   MetalJet
_diffrn_source_current           2.86
_diffrn_source_power             0.19931339999999997
_diffrn_source_type              'Liquid Metal source'
_diffrn_source_voltage           69.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.020
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.5374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1346 before and 0.0917 after correction.
The Ratio of minimum to maximum transmission is 0.7154.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    2.081
_exptl_crystal_description       needle
_exptl_crystal_F_000             2316
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Flack x determined using 575 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         2484
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0745P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1305
_reflns_Friedel_coverage         0.606
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                1822
_reflns_number_total             2484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05850b2.cif
_cod_data_source_block           29150003_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7131208.cif.
;
_cod_original_cell_volume        3634.2(7)
_cod_original_sg_symbol_Hall     'P 61 2 (0 0 -1)'
_cod_database_code               7131208
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.689
_shelx_estimated_absorpt_t_min   0.623
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2-C8 = C8-C7 = C7-C6 = C6-C5 = N1-C1
 1.5 with sigma of 0.005
 C4-C3 = C3-C2
 1.5 with sigma of 0.005
 N2-C4 = N1-C2
 1.45 with sigma of 0.005
 N2-C7
 2.4 with sigma of 0.005
 C5-C8
 2.4 with sigma of 0.005
 C7-C5
 2.4 with sigma of 0.005
 C8-C6
 2.5 with sigma of 0.005
 N2-C6
 2.4 with sigma of 0.005
 C4-C2
 2.5 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C4 \\sim N1 \\sim C1 \\sim C2 \\sim C5 \\sim C3 \\sim N2 \\sim C6 \\sim C8
\\sim C7: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
4. Others
 Fixed Sof: N1(0.5) C5(0.5) N2(0.5) C4(0.5) H4A(0.5) H4B(0.5) C3(0.5) H3A(0.5)
 H3B(0.5) C2(0.5) H2A(0.5) H2B(0.5) C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C6(0.5)
 H6A(0.5) H6B(0.5) C7(0.5) H7A(0.5) H7B(0.5) C8(0.5) H8A(0.5) H8B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C3(H3A,H3B), C2(H2A,H2B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B)
5.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              12288
_shelx_hkl_checksum              34137
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU