Diverse tetrahedral tetrazolate frameworks with N-rich surface.
Tang, Yu-Huan; Wang, Fei; Liu, Jin-Xiu; Zhang, Jian; Chemical communications (Cambridge, England) 52 (2016) 5625–5628; doi:10.1039/c6cc00589f

data_7118931
_publ_section_title
;
 Diverse tetrahedral tetrazolate frameworks with N-rich surface.
;
_journal_issue                   32
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5625
_journal_page_last               5628
_journal_paper_doi               10.1039/c6cc00589f
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C6 H9 N12 O8 S2 Zn2, 3(C4 H12 N)'
_chemical_formula_sum            'C18 H45 N15 O8 S2 Zn2'
_chemical_formula_weight         794.55
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-03-01
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2016-03-15 deposited with the CCDC.
2016-03-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7886(13)
_cell_length_b                   15.9425(9)
_cell_length_c                   16.3286(7)
_cell_measurement_reflns_used    3134
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.8700
_cell_measurement_theta_min      2.8320
_cell_volume                     4110.1(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2083
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0972
_diffrn_reflns_av_unetI/netI     0.1171
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11870
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         2.495
_exptl_absorpt_coefficient_mu    1.321
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_description       block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;
 ?
;
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 1144 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         7128
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0793
_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^)+(0.0950P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1912
_refine_ls_wR_factor_ref         0.2203
_reflns_Friedel_coverage         0.773
_reflns_Friedel_fraction_full    0.970
_reflns_Friedel_fraction_max     0.970
_reflns_number_gt                4516
_reflns_number_total             7128
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc00589f3.cif
_cod_data_source_block           ttf_5
_cod_depositor_comments
'Adding full bibliography for 7118929--7118932.cif.'
_cod_database_code               7118931
_shelx_estimated_absorpt_t_max   0.837
_shelx_estimated_absorpt_t_min   0.826
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H) groups, All N(H,H) groups
2. Restrained distances
 C7-C8 = C9-C10 = C11_$1-C12_$1 = C13_$1-C14_$1 = C15_$2-C16_$2 = C17_$2-C18_$2
 1.55 with sigma of 0.001
 C8-C9 = C12_$1-C13_$1 = C16_$2-C17_$2
 2.31 with sigma of 0.001
 N13-C8 = N13-C9 = N14_$1-C12_$1 = N14_$1-C13_$1 = N15_$2-C16_$2 = N15_$2-C17_$2
 1.5 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(N14)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq,
Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2)
\\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O7) \\sim Ueq,
Uanis(O6) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 N13, C9, C8, C10, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N14, C12, C13, C11, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17, N15, C16, C18, C15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Riding coordinates:
 C7(H7A,H7B,H7C)
5.b Secondary CH2 refined with riding coordinates:
 N13(H13A,H13B), N14(H14A,H14B), C12(H12A,H12B), C9(H9A,H9B), N15(H15A,H15B),
 C17(H17A,H17B), C16(H16A,H16B), C13(H13C,H13D), C8(H8A,H8B)
5.c Me refined with riding coordinates:
 C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C2(H2A,H2B,H2C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C15(H15C,H15D,H15E), C14(H14C,H14D,H14E), C18(H18A,H18B,
 H18C)
;
_shelx_res_checksum              60630
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'