Supramolecular assemblies of benzene-1,3,5-tricarboxylic acid and 3,5-substituted pyrazoles: formation and structural analysis
Singh, Udai P.; Tomar, Kapil; Kashyap, Sujata; CrystEngComm 17 (2015) 1421–; doi:10.1039/C4CE02117G

data_7219270
_publ_section_title
;
 Supramolecular assemblies of benzene-1,3,5-tricarboxylic acid and
 3,5-substituted pyrazoles: formation and structural analysis
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              1421
_journal_paper_doi               10.1039/C4CE02117G
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C9 H6 O6, C9 H5 O6, C9.92 H19 N2, 0.06(O)'
_chemical_formula_sum            'C27.92 H30 N2 O12.06'
_chemical_formula_weight         586.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-10-21 deposited with the CCDC.
2014-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                94.839(15)
_cell_angle_beta                 104.698(14)
_cell_angle_gamma                104.297(14)
_cell_formula_units_Z            2
_cell_length_a                   10.037(3)
_cell_length_b                   10.936(3)
_cell_length_c                   14.655(4)
_cell_measurement_reflns_used    102
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.78
_cell_measurement_theta_min      2.34
_cell_volume                     1489.1(7)
_computing_cell_refinement       'Bruker Kappa Apex'
_computing_data_collection       'Bruker Kappa Apex'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25830
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             616.0
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         5233
_refine_ls_number_restraints     384
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.7687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1611
_refine_ls_wR_factor_ref         0.1837
_reflns_number_gt                3362
_reflns_number_total             5233
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce02117g2.cif
_cod_data_source_block           ups475kt3_0m
_cod_depositor_comments
'Adding full bibliography for 7219268--7219274.cif.'
_cod_database_code               7219270