A Conformationally Persistent Pseudo-bicyclic Guanidinium for Anion Coordination As Stabilized by Dual Intramolecular Hydrogen Bonds
Seipp, Charles Aaron; Williams, Neil J.; Bryantsev, Vyacheslav; Custelcean, Radu; Moyer, Bruce A.; RSC Adv.  (2015) –; doi:10.1039/C5RA21864K

data_7223378
_publ_section_title
;
 A Conformationally Persistent Pseudo-bicyclic Guanidinium for Anion
 Coordination As Stabilized by Dual Intramolecular Hydrogen Bonds
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA21864K
_journal_year                    2015
_chemical_formula_sum            'C24 H24 N10 O10 S'
_chemical_formula_weight         644.60
_chemical_name_systematic        'N,N'-bis(2-pyridyl)guanidinium hemisulfate'
_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
_audit_update_record
;
2015-06-03 deposited with the CCDC.
2015-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 108.610(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.585(4)
_cell_length_b                   16.445(4)
_cell_length_c                   11.369(3)
_cell_measurement_temperature    120(2)
_cell_volume                     3115.8(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7960
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_T_max  0.9880
_exptl_absorpt_correction_T_min  0.9517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1336
_exptl_crystal_recrystallization_method
'Slow diffusion of diethyl ether into methanol'
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.312
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         2747
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1145
_refine_ls_R_factor_gt           0.0959
_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^)+(0.1914P)^2^+7.2401P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2831
_refine_ls_wR_factor_ref         0.3015
_reflns_number_gt                2110
_reflns_number_total             2747
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra21864k2.cif
_cod_data_source_block           c:\frames\636\work\636s
_cod_original_cell_volume        3115.9(13)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7223378