A strategy for the propagation of hydrogen-bonding in bicyclic guanidinium salts
Khalaf, Majid S.; Oakley, Sarah H.; Coles, Martyn P.; Hitchcock, Peter B.; CrystEngComm  (2008) –; doi:10.1039/b811191j

data_7202375
_publ_section_title
;
 A strategy for the propagation of hydrogen-bonding in bicyclic
 guanidinium salts
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/b811191j
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C5 H10 N3, Cl'
_chemical_formula_sum            'C5 H10 Cl N3'
_chemical_formula_weight         147.61
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2008-05-14T13:56:58-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 101.462(2)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   13.5414(5)
_cell_length_b                   13.5232(5)
_cell_length_c                   16.1341(5)
_cell_measurement_reflns_used    11145
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     2895.60(18)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.65211E-1
_diffrn_orient_matrix_UB_12      -0.122747E-1
_diffrn_orient_matrix_UB_13      -0.184232E-1
_diffrn_orient_matrix_UB_21      0.101126E-1
_diffrn_orient_matrix_UB_22      0.729004E-1
_diffrn_orient_matrix_UB_23      -0.45407E-2
_diffrn_orient_matrix_UB_31      0.363721E-1
_diffrn_orient_matrix_UB_32      0.17385E-2
_diffrn_orient_matrix_UB_33      0.603282E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.066
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18447
_diffrn_reflns_theta_full        26.03
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         3.42
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.442
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.24
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         5654
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+1.7070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.101
_refine_ls_wR_factor_ref         0.1155
_reflns_number_gt                3939
_reflns_number_total             5654
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b811191j.txt
_cod_data_source_block           may608
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7202375