Water of Hydration in 2:1 Hydrogen-Bonded Complexes between 1,5,7-Triazabicyclo[4.4.0]dec-5-ene and Dicarboxylic Acids
Yadav, Vitthal N.; Görbitz, Carl Henrik; Crystal Growth & Design 13 (2013) 2174–; doi:10.1021/cg400250n

data_4507744
_publ_section_title
;
 Water of Hydration in 2:1 Hydrogen-Bonded Complexes between
 1,5,7-Triazabicyclo[4.4.0]dec-5-ene and Dicarboxylic Acids
;
_journal_issue                   5
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2174
_journal_paper_doi               10.1021/cg400250n
_journal_volume                  13
_journal_year                    2013
_chemical_formula_moiety         'C7 H3 N O4, 2(C7 H14 N3), 4(H2 O)'
_chemical_formula_sum            'C21 H39 N7 O8'
_chemical_formula_weight         517.59
_chemical_name_systematic
;
bis(1,3,4,6,7,8-hexahydro-2H-pyrimido[1,2-a]pyrimidinium.
pyridine-3,5-dicarboxylate tetrahydrate'
;
_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
;
2013-01-24 # Formatted by publCIF
;
_cell_angle_alpha                84.407(11)
_cell_angle_beta                 87.349(13)
_cell_angle_gamma                73.631(11)
_cell_formula_units_Z            2
_cell_length_a                   7.454(7)
_cell_length_b                   10.516(10)
_cell_length_c                   16.998(16)
_cell_measurement_reflns_used    1742
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      25.98
_cell_measurement_theta_min      2.26
_cell_volume                     1272(2)
_computing_cell_refinement       'SAINT-Plus (Bruker,2007)'
_computing_data_collection       APEX2(Bruker2007)
_computing_data_reduction        'SAINT-Plus (Bruker,2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      105(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0977
_diffrn_reflns_av_sigmaI/netI    0.1358
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13543
_diffrn_reflns_theta_full        26.91
_diffrn_reflns_theta_max         26.91
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.251
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5168
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1604
_refine_ls_R_factor_gt           0.0843
_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^)+(0.0665P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1511
_refine_ls_wR_factor_ref         0.1784
_reflns_number_gt                2982
_reflns_number_total             5512
_reflns_threshold_expression     >2sigma(I)
_publcif_info_exptl_table_max_cols 6
_cod_data_source_file            cg400250n_si_003.cif
_cod_data_source_block           vny159lt2
_cod_database_code               4507744