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_7202373
_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         'C7 H14 Br1 N3'
_chemical_formula_sum            'C7 H14 Br N3'
_chemical_formula_weight         220.12
_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             2003-08-20T13:46:46-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 99.411(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.8903(3)
_cell_length_b                   8.8030(4)
_cell_length_c                   15.1958(8)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.713
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     909.30(7)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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      -0.75303E-2
_diffrn_orient_matrix_UB_12      -0.480842E-1
_diffrn_orient_matrix_UB_13      0.589679E-1
_diffrn_orient_matrix_UB_21      0.11782
_diffrn_orient_matrix_UB_22      0.594907E-1
_diffrn_orient_matrix_UB_23      0.278455E-1
_diffrn_orient_matrix_UB_31      -0.877707E-1
_diffrn_orient_matrix_UB_32      0.839832E-1
_diffrn_orient_matrix_UB_33      0.140371E-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  0.1095
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9052
_diffrn_reflns_theta_full        24.68
_diffrn_reflns_theta_max         24.68
_diffrn_reflns_theta_min         3.7
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    4.464
_exptl_absorpt_correction_T_max  0.5781
_exptl_absorpt_correction_T_min  0.3958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.025
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     108
_refine_ls_number_reflns         1531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0423P)^2^+2.1938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1144
_reflns_number_gt                1201
_reflns_number_total             1531
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b811191j.txt
_cod_data_source_block           1b-aug503
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C7 H14 Br1 N3'
_cod_database_code               7202373