N-Methylated Diphenylguanidines: Conformations, Propeller-Type Molecular Chirality, and Construction of Water-Soluble Oligomers with Multilayered Aromatic Structures
Aya Tanatani; Kentaro Yamaguchi; Isao Azumaya; Ryuuta Fukutomi; Koichi Shudo; Hiroyuki Kagechika; Journal of the American Chemical Society 120 (1998) 6433–6442; doi:10.1021/ja9806534

data_4116752
_publ_section_title
;
 N-Methylated Diphenylguanidines: Conformations, Propeller-Type Molecular
 Chirality, and Construction of Water-Soluble Oligomers with Multilayered
 Aromatic Structures
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6433
_journal_page_last               6442
_journal_paper_doi               10.1021/ja9806534
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C15 H18 Br N3'
_chemical_formula_weight         320.23
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Fri Jan  9 13:58:12 1998'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                91.85(2)
_cell_angle_beta                 94.99(2)
_cell_angle_gamma                65.14(1)
_cell_formula_units_Z            4
_cell_length_a                   13.034(3)
_cell_length_b                   13.216(4)
_cell_length_c                   9.711(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      21.8
_cell_measurement_theta_min      20.0
_cell_volume                     1512.0(7)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC5S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.05564
_diffrn_orient_matrix_UB_12      -0.07670
_diffrn_orient_matrix_UB_13      -0.02323
_diffrn_orient_matrix_UB_21      0.01916
_diffrn_orient_matrix_UB_22      -0.01842
_diffrn_orient_matrix_UB_23      0.10072
_diffrn_orient_matrix_UB_31      -0.06111
_diffrn_orient_matrix_UB_32      -0.02706
_diffrn_orient_matrix_UB_33      -0.00119
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku sealed tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_av_sigmaI/netI    0.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4723
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         0.00
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        -0.06
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.621
_exptl_absorpt_correction_T_max  1.301
_exptl_absorpt_correction_T_min  0.630
_exptl_absorpt_correction_type   '\DF (DIFABS; Walker & Stuart, 1983)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             656.00
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.76
_refine_diff_density_min         -1.03
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   5.870
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     471
_refine_ls_number_reflns         3427
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0790
_refine_ls_shift/esd_max         7.5690
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.1000
_reflns_number_observed          3427
_reflns_number_total             4493
_reflns_observed_criterion       >3.0sigma(I)
_cod_data_source_file            ja9806534_06.cif
_cod_data_source_block           Compound_4b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00000|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) + 0.00000|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1512.1(6)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C15 H18 Br N3 '
_cod_database_code               4116752