Pyridine–Urea-Based Anion Receptor: Formation of Cyclic Sulfate–Water Hexamer and Dihydrogen Phosphate–Water Trimer in Hydrophobic Environment
Hoque, Md. Najbul; Basu, Arghya; Das, Gopal; Crystal Growth & Design 14 (2014) 6–; doi:10.1021/cg4015724

data_4510018
_publ_section_title
;
 Pyridine--Urea-Based Anion Receptor: Formation of Cyclic Sulfate--Water
 Hexamer and Dihydrogen Phosphate--Water Trimer in Hydrophobic Environment
;
_journal_issue                   1
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              6
_journal_paper_doi               10.1021/cg4015724
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C13 H14 N6 O, 2(Cl O4), 2(H2 O)'
_chemical_formula_sum            'C13 H18 Cl2 N6 O11'
_chemical_formula_weight         505.23
_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
_cell_angle_alpha                79.566(3)
_cell_angle_beta                 80.063(3)
_cell_angle_gamma                70.872(3)
_cell_formula_units_Z            2
_cell_length_a                   7.5545(4)
_cell_length_b                   8.7273(4)
_cell_length_c                   16.7176(9)
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.89
_cell_measurement_theta_min      2.49
_cell_volume                     1016.49(9)
_computing_cell_refinement       'Bruker SAINT, 1998'
_computing_data_collection       'Bruker SMART, 1998'
_computing_data_reduction        'Bruker SAINT, 1998'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0775
_diffrn_reflns_av_sigmaI/netI    0.0597
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9861
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2007)''
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Needle type'
_exptl_crystal_F_000             520.0
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         5012
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0623
_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^)+(0.1400P)^2^+0.0200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1987
_refine_ls_wR_factor_ref         0.2118
_reflns_number_gt                2962
_reflns_number_total             5012
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg4015724_si_002.cif
_cod_data_source_block           LH2-2ClO4-2H2O
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4510018