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_4507745
_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         '2(C7 H14 N3), C8 H4 O4, 3(H2 O)'
_chemical_formula_sum            'C22 H38 N6 O7'
_chemical_formula_weight         498.57
_chemical_name_common
Di(1,5,7-triazabicyclo[4.4.0]dec-5-ene).Phthalatetrihydrate
_chemical_name_systematic
;
1,2,benzenedicarboxylate.bis(1,3,4,6,7,8-hexahydro-2H-pyrimido
[1,2-a]pyrimidinium)trihydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2012-06-01 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 107.986(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5739(12)
_cell_length_b                   30.821(4)
_cell_length_c                   9.7863(13)
_cell_measurement_reflns_used    8685
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      28.64
_cell_measurement_theta_min      2.29
_cell_volume                     2459.7(6)
_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 0.990
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and \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  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            21942
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         28.94
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  0.9899
_exptl_absorpt_correction_T_min  0.964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         5998
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0485P)^2^+1.0027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.1028
_reflns_number_gt                4849
_reflns_number_total             6509
_reflns_threshold_expression     >2sigma(I)
_publcif_info_exptl_table_max_cols 6
_cod_data_source_file            cg400250n_si_004.cif
_cod_data_source_block           vny124
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4507745