New complexes constructed from in situ nitration of (1H-tetrazol-5-yl)phenol: synthesis, structures and properties
Du, Ceng-Ceng; Wang, Xin-Fang; Zhou, Sheng-Bin; Wang, Duo-Zhi; Jia, Dianzeng; CrystEngComm  (2017) –; doi:10.1039/C7CE00753A

data_7229372
_publ_section_title
;
 New complexes constructed from in situ nitration of
 (1H-tetrazol-5-yl)phenol: synthesis, structures and properties
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00753A
_journal_year                    2017
_chemical_formula_moiety         '0.25(C56 H24 N48 O48 Zn12), O'
_chemical_formula_sum            'C14 H8 N12 O13 Zn3'
_chemical_formula_weight         748.43
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-08-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-10-18 deposited with the CCDC.
2017-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.331(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1335(8)
_cell_length_b                   7.9549(5)
_cell_length_c                   20.8717(14)
_cell_measurement_reflns_used    3710
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.08
_cell_measurement_theta_min      2.98
_cell_volume                     2227.5(2)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            6918
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.074
_diffrn_reflns_theta_max         25.074
_diffrn_reflns_theta_min         2.056
_exptl_absorpt_coefficient_mu    3.305
_exptl_absorpt_correction_T_max  0.5877
_exptl_absorpt_correction_T_min  0.5301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.232
_exptl_crystal_description       block
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         1984
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0245
_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^)+(0.0356P)^2^+5.7500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0682
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1829
_reflns_number_total             1984
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00753a2.cif
_cod_data_source_block           1
_cod_original_cell_volume        2227.6(2)
_cod_database_code               7229372
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.588
_shelx_estimated_absorpt_t_min   0.530
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
2. Restrained distances
 N6-O5A = N6-O5B = N6-O6A = N6-O6B
 1.22 with sigma of 0.02
 O1-H1
 0.84 with sigma of 0.02
 C4-O5A \\sim C4-O5B \\sim C4-O6A \\sim C4-O6B
 with sigma of 0.01
3. Rigid bond restraints
 N6, O5A, O5B, O6A, O6B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
N6 \\sim O5A \\sim O5B \\sim O6A \\sim O6B: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
5. Others
 Sof(O5B)=Sof(O6B)=1-FVAR(1)
 Sof(O5A)=Sof(O6A)=FVAR(1)
 Fixed Sof: O7(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7)
;
_olex2_submission_special_instructions 'No special instructions were received'