Structural Study of Salicylic Acid Salts of a Series of Azacycles and Azacrown Ethers†
Fonari, Marina S.; Ganin, Eduard V.; Basok, Stepan S.; Lyssenko, Konstantin A.; Zaworotko, Michael J.; Kravtsov, Victor Ch.; Crystal Growth & Design 10 (2010) 5210–; doi:10.1021/cg101002x

data_4502089
_publ_section_title
;
 Structural Study of Salicylic Acid Salts of a Series of Azacycles and
 Azacrown Ethers&#x2020;
;
_journal_issue                   12
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              5210
_journal_paper_doi               10.1021/cg101002x
_journal_volume                  10
_journal_year                    2010
_chemical_formula_moiety         'C12 H28 N2 O4, 2(C7 H5 O3), 3(H2 O)'
_chemical_formula_sum            'C26 H44 N2 O13'
_chemical_formula_weight         592.63
_chemical_name_common
; 
 7,16-Diazonia-18-crown-6 bis(salicylate) trihydrate
;
_chemical_name_systematic
; 
 1,4,10,13-tetraoxa-7,16-diazoniacyclooctadecane 
bis(2-hydroxybenzoate) trihydrate
;
_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                98.175(4)
_cell_angle_beta                 90.721(2)
_cell_angle_gamma                111.355(3)
_cell_formula_units_Z            2
_cell_length_a                   9.434(2)
_cell_length_b                   12.587(3)
_cell_length_c                   13.843(2)
_cell_measurement_temperature    100(2)
_cell_volume                     1511.7(5)
_computing_cell_refinement       'Bruker SMART-APEX CCD'
_computing_data_collection       'Bruker SMART-APEX CCD'
_computing_data_reduction        'Bruker SMART-APEX CCD'
_computing_molecular_graphics    Mercury
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0878
_diffrn_reflns_av_sigmaI/netI    0.1606
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8062
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         5352
_refine_ls_number_restraints     276
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.1810
_refine_ls_R_factor_gt           0.0923
_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^)+(0.1234P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2341
_refine_ls_wR_factor_ref         0.2700
_reflns_number_gt                2221
_reflns_number_total             5352
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg101002x_si_001.cif
_cod_data_source_block           vk2003c3
_cod_original_cell_volume        1511.7(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4502089