Three-Component Carboxylic Acid−Bipyridine Lattice Inclusion Host. Supramolecular Synthesis of Ternary Cocrystals
Bhogala, Balakrishna R.; Basavoju, Srinivas; Nangia, Ashwini; Crystal Growth & Design 5 (2005) 1683–; doi:10.1021/cg058012p

data_4505255
_publ_section_title
;
 Three-Component Carboxylic Acid&#x2212;Bipyridine Lattice Inclusion Host.
 Supramolecular Synthesis of Ternary Cocrystals
;
_journal_issue                   5
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1683
_journal_paper_doi               10.1021/cg058012p
_journal_volume                  5
_journal_year                    2005
_chemical_formula_moiety         'C9 H12 O6, 0.5(C12 H10 N2 O2), 0.5(C10 H8 N2)'
_chemical_formula_sum            'C20 H21 N2 O7'
_chemical_formula_weight         401.39
_chemical_melting_point          531
_chemical_name_systematic
; 
   cis,cis-1,3,5-cyclohexanetricarboxylic acid 
- 1,2-bis(4-pyridyl-N-oxy)ethylene - 4,4'-bipyridine
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.73(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.1002(12)
_cell_length_b                   12.531(3)
_cell_length_c                   25.138(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.6
_cell_volume                     1917.5(7)
_computing_cell_refinement       'CAD4 data collection software'
_computing_data_collection       'CAD4 data collection software'
_computing_data_reduction        'WinGx Version 1.64.05'
_computing_molecular_graphics    'PLUTON (Spek, 1992)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  Enraf-Nonius-MACH3
_diffrn_measurement_method       '\w 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  0.0163
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            4790
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.62
_diffrn_standards_interval_count 150
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.39
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             844.0
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         4382
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.0618
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0854P)^2^+1.0528P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1488
_refine_ls_wR_factor_ref         0.1888
_reflns_number_gt                2559
_reflns_number_total             4384
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg058012p_s4.cif
_cod_data_source_block           (H3CTA).(BPENO)0.5.(bipy)0.5
_cod_original_cell_volume        1917.6(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4505255