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_7229373
_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         'C14 H4 Cu3 N12 O12, 0.5(O)'
_chemical_formula_sum            'C14 H12 Cu3 N12 O13'
_chemical_formula_weight         746.96
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_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                113.73(4)
_cell_angle_beta                 102.22(4)
_cell_angle_gamma                104.23(4)
_cell_formula_units_Z            2
_cell_length_a                   10.243(13)
_cell_length_b                   10.444(13)
_cell_length_c                   11.595(14)
_cell_measurement_reflns_used    535
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.08
_cell_measurement_theta_min      2.52
_cell_volume                     1031(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      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0946
_diffrn_reflns_av_unetI/netI     0.1578
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6550
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.187
_diffrn_reflns_theta_max         25.187
_diffrn_reflns_theta_min         2.048
_exptl_absorpt_coefficient_mu    3.174
_exptl_absorpt_correction_T_max  0.5989
_exptl_absorpt_correction_T_min  0.5419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             726
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.915
_refine_diff_density_min         -2.025
_refine_diff_density_rms         0.261
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         3644
_refine_ls_number_restraints     994
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.1544
_refine_ls_R_factor_gt           0.0738
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1659P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2425
_refine_ls_wR_factor_ref         0.2938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1956
_reflns_number_total             3644
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00753a2.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7229373
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.599
_shelx_estimated_absorpt_t_min   0.542
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 Cu1, O12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N11, O9, O10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C10 \\sim C11
\\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim N10 \\sim N9 \\sim N12
\\sim N11 \\sim N1 \\sim N2 \\sim N3 \\sim N4 \\sim N5 \\sim N6 \\sim N7 \\sim
N8 \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8
\\sim O9 \\sim O10 \\sim O11 \\sim O12 \\sim O13: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(N4) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(O12) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: O13(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C12(H12), C16(H16)
5.b Fitted hexagon refined as free rotating group:
 C2(C3,C4,C5,C6,C7), C11(C12,C13,C14,C15,C16)
;
_olex2_submission_special_instructions 'No special instructions were received'