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_7223379
_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            'C11 H19 N5 O5.5 S0.5'
_chemical_formula_weight         325.34
_chemical_name_systematic        'N,N'-bis(2-pyridyl)guanidinium hemisulfate'
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.941(4)
_cell_length_b                   8.827(2)
_cell_length_c                   20.578(5)
_cell_measurement_temperature    173(2)
_cell_volume                     3077.2(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  Bruker
_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  0.1532
_diffrn_reflns_av_sigmaI/netI    0.1005
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17227
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    0.177
_exptl_absorpt_correction_T_max  0.9982
_exptl_absorpt_correction_T_min  0.9167
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1376
_exptl_crystal_recrystallization_method 'Slow evaporation from water'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         2719
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.1374
_refine_ls_R_factor_gt           0.0672
_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^)+(0.0875P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1840
_reflns_number_gt                1471
_reflns_number_total             2719
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra21864k2.cif
_cod_data_source_block           c:\frames\684\work\pbcn
_cod_original_sg_symbol_H-M      Pbcn
_cod_original_formula_sum        'C11 H19 N5 O5.50 S0.50'
_cod_database_code               7223379