Synthesis and characterization of a layered aluminosilicate NUD-11 and its transformation to a 3D stable zeolite.
Zi, Wen-Wen; Zhang, Jun; Cai, Xian-Shu; Jiao, Feng; Du, Hong-Bin; Dalton transactions (Cambridge, England : 2003) 49 (2020) 11682–11688; doi:10.1039/d0dt02449j

data_7704958
_publ_section_title
;
 Synthesis and characterization of a layered aluminosilicate NUD-11 and
 its transformation to a 3D stable zeolite.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11682
_journal_page_last               11688
_journal_paper_doi               10.1039/d0dt02449j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'O38 Si18, 5(C9 H11 N2), F, 2(H2 O)'
_chemical_formula_sum            'C45 H59 F N10 O40 Si18'
_chemical_formula_weight         1904.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-06-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-21 deposited with the CCDC.	2020-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.264(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.767(4)
_cell_length_b                   26.561(6)
_cell_length_c                   7.380(2)
_cell_measurement_reflns_used    1327
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.43
_cell_measurement_theta_min      2.64
_cell_volume                     3089.9(13)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1391
_diffrn_reflns_av_unetI/netI     0.1827
_diffrn_reflns_Laue_measured_fraction_full 0.951
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9208
_diffrn_reflns_point_group_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.456
_diffrn_reflns_theta_min         2.584
_exptl_absorpt_coefficient_mu    0.497
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.047
_exptl_crystal_description       slice
_exptl_crystal_F_000             1960
_refine_diff_density_max         0.944
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         3399
_refine_ls_number_restraints     278
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1889
_refine_ls_R_factor_gt           0.0923
_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^)+(0.1339P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2111
_refine_ls_wR_factor_ref         0.2606
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1708
_reflns_number_total             3399
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02449j2.cif
_cod_data_source_block           a_a
_cod_depositor_comments          'Adding full bibliography for 7704958.cif.'
_cod_database_code               7704958
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N3-C6 = N3-C13 = C13-N2 = C11-C6 = C11-N2
 1.45 with sigma of 0.01
 C13-C11 = C13-C6
 2.4 with sigma of 0.02
 C11-C13
 2.4 with sigma of 0.02
 C11-N3
 2.4 with sigma of 0.02
 N3-N2 = C6-N2
 2.4 with sigma of 0.02
 C13-C12
 2.5 with sigma of 0.02
 C11-C12
 2.5 with sigma of 0.02
 C14-C6
 2.5 with sigma of 0.02
 C14-C13
 2.5 with sigma of 0.02
 C14-N3 = N2-C12
 1.5 with sigma of 0.02
 N2-C12 = N3-C14
 1.5 with sigma of 0.01
3. Restrained planarity
 C6, C12, N2, C11, C13, C10, N3, C9, C7, C14, C8
 with sigma of 0.01
 N3, C12, N2, C11, C13, C10, C6, C14, C9, C7, C8
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C12 \\sim N2 \\sim C11 \\sim C13 \\sim C10 \\sim C6 \\sim N3 \\sim C9 \\sim C7
\\sim C14 \\sim C8: within 2A with sigma of 0.02 and sigma for terminal atoms
of 0.02
Uanis(O10) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C6) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C12) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(N3) \\sim Ueq,
Uanis(C9) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C14) \\sim
Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(O11) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 C12, N2, C11, C13, C10, C6, N3, C9, C7, C14, C8
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
6. Others
 Fixed Sof: C12(0.75) H12A(0.75) H12B(0.75) H12C(0.75) N2(0.75) C7(0.75)
 H7(0.75) C8(0.75) H8(0.75) C9(0.75) H9(0.75) C10(0.75) H10(0.75) C11(0.75)
 C6(0.75) C13(0.75) H13(0.75) N3(0.75) C14(0.75) H14A(0.75) H14B(0.75)
 H14C(0.75) F1(0.25) O11(0.5) H11A(0.5) H11B(0.5)
 Fixed X: F1(-0.18683) O11(-0.101739)
 Fixed Y: F1(-0.49524) O11(-0.52914)
 Fixed Z: F1(-0.62197) O11(-0.71604)
7.a Riding coordinates:
 C5(H5A,H5B,H5C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), O11(H11A,H11B)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13)
7.c Fitted hexagon refined as free rotating group:
 C7(C8,C9,C10,C11,C6)
;
_shelx_res_checksum              46441
_olex2_submission_special_instructions 'No special instructions were received'