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_7229377
_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 H18 Co N12 O16'
_chemical_formula_sum            'C14 H18 Co N12 O16'
_chemical_formula_weight         669.30
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-10-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 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                75.352(8)
_cell_angle_beta                 78.014(12)
_cell_angle_gamma                67.635(12)
_cell_formula_units_Z            1
_cell_length_a                   6.688(3)
_cell_length_b                   7.946(3)
_cell_length_c                   12.609(5)
_cell_measurement_reflns_used    4876
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      29.754
_cell_measurement_theta_min      2.560
_cell_volume                     594.9(4)
_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      273.15
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3793
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.032
_diffrn_reflns_theta_max         25.032
_diffrn_reflns_theta_min         1.682
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_correction_T_min  0.835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_description       block
_exptl_crystal_F_000             321
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.233
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         2077
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1110
_refine_ls_R_factor_gt           0.0715
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+16.3831P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2602
_refine_ls_wR_factor_ref         0.2648
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1749
_reflns_number_total             2077
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00753a2.cif
_cod_data_source_block           3
_cod_database_code               7229377
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.840
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O7(H7A,H7B), O8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), N1(H1)
;
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20