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_4510808
_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(C12 H12 N2), 2(H2 O)'
_chemical_formula_sum            'C63 H64 N O8'
_chemical_formula_weight         963.15
_chemical_name_systematic
; 
 ? 
;
_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                 118.325(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.315(10)
_cell_length_b                   18.540(5)
_cell_length_c                   25.319(8)
_cell_measurement_reflns_used    14692
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      1.53
_cell_volume                     12527(7)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_sigmaI/netI    0.1074
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            25148
_diffrn_reflns_theta_full        25.33
_diffrn_reflns_theta_max         25.33
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.9888
_exptl_absorpt_correction_T_min  0.9855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.021
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4104
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.342
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         11311
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.382
_refine_ls_R_factor_all          0.1896
_refine_ls_R_factor_gt           0.1201
_refine_ls_shift/su_max          0.001
_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^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2907
_refine_ls_wR_factor_ref         0.3192
_reflns_number_gt                5596
_reflns_number_total             11311
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            HPB-bipy-eta.cif
_cod_data_source_block           HPB-bipy-eta
_cod_original_cell_volume        12526(7)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4510808