Observation of a Persistent Supramolecular Synthon Involving Carboxyl Groups and H2O That Guides the Formation of Polycatenated Co-crystals of a Tritopic Carboxylic Acid and Bis(pyridyls)
Wang, Lian-Cheng; Sun, Junliang; Huang, Zhi-Tang; Zheng, Qi-Yu; Crystal Growth & Design 13 (2013) 1–; doi:10.1021/cg301015a

data_4510807
_publ_section_title
;
 Observation of a Persistent Supramolecular Synthon Involving Carboxyl
 Groups and H2O That Guides the Formation of Polycatenated Co-crystals of
 a Tritopic Carboxylic Acid and Bis(pyridyls)
;
_journal_issue                   1
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1
_journal_paper_doi               10.1021/cg301015a
_journal_volume                  13
_journal_year                    2013
_chemical_formula_moiety
'C57 H54 O6, 0.5(C10 H8 N4), 2(C3 H6 O), 2(H2 O)'
_chemical_formula_sum            'C68 H74 N2 O10'
_chemical_formula_weight         1079.29
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 122.213(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.120(6)
_cell_length_b                   18.155(3)
_cell_length_c                   25.759(5)
_cell_measurement_reflns_used    10750
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      1.31
_cell_volume                     12313(4)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0674
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            24919
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  0.9885
_exptl_absorpt_correction_T_min  0.9847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4608
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.867
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         10818
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.1181
_refine_ls_R_factor_gt           0.0976
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0944P)^2^+32.5056P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2318
_refine_ls_wR_factor_ref         0.2461
_reflns_number_gt                8718
_reflns_number_total             10818
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            HPB-azopy.cif
_cod_data_source_block           HPB-azopy
_cod_original_cell_volume        12314(4)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4510807