Syntheses, Conformations, and Basicities of Bicyclic Triamines
Thomas W. Bell; Heung-Jin Choi; William Harte; Michael G. B. Drew; Journal of the American Chemical Society 125 (2003) 12196–12210; doi:10.1021/ja030236d

data_4114214
_publ_section_title
;
 Syntheses, Conformations, and Basicities of Bicyclic Triamines
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12196
_journal_page_last               12210
_journal_paper_doi               10.1021/ja030236d
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C14 H28 I N3'
_chemical_formula_weight         375.10
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.000(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.145(9)
_cell_length_b                   13.984(12)
_cell_length_c                   15.698(14)
_cell_measurement_temperature    293(2)
_cell_volume                     1680(3)
_computing_cell_refinement       'Stoe Software'
_computing_data_collection       'Stoe Software'
_computing_data_reduction        'Stoe Software'
_computing_molecular_graphics    PLATON(Spek,1994)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Stoe Stadi 2circle diffractometer'
_diffrn_measurement_method       'variable width w scan'
_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  0.0857
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            2859
_diffrn_reflns_theta_max         25.11
_diffrn_reflns_theta_min         3.12
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 20
_diffrn_standards_number         '4 per layer'
_exptl_absorpt_coefficient_mu    1.974
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.417
_exptl_absorpt_correction_type   DIFABS
_exptl_crystal_density_diffrn    2.381
_exptl_crystal_F_000             1212
_refine_diff_density_max         1.32
_refine_diff_density_min         -1.23
_refine_ls_extinction_coef       0.0104(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2869
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.1750
_refine_ls_R_factor_gt           0.0730
_refine_ls_shift/su_max          0.104
_refine_ls_shift/su_mean         0.082
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/[\s^2^(Fo^2^)+(0.003*Fo^2)]
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.1750
_reflns_number_gt                1812
_reflns_number_total             2869
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja030236d_1.cif
_cod_data_source_block           16HI
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.003*Fo^2)]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w=1/[\s^2^(Fo^2^)+(0.003*Fo^2)]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4114214