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_4116748
_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            'C13 H13 N3'
_chemical_formula_weight         211.27
_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'
_audit_creation_date             'Fri Jan  9 14:00:04 1998'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 96.66(1)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.906(2)
_cell_length_b                   12.342(1)
_cell_length_c                   21.335(2)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      15.7
_cell_measurement_theta_min      14.1
_cell_volume                     2329.3(6)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/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 AFC7S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.01580
_diffrn_orient_matrix_UB_12      0.08019
_diffrn_orient_matrix_UB_13      -0.00205
_diffrn_orient_matrix_UB_21      0.02721
_diffrn_orient_matrix_UB_22      0.00494
_diffrn_orient_matrix_UB_23      0.04672
_diffrn_orient_matrix_UB_31      0.10859
_diffrn_orient_matrix_UB_32      0.01048
_diffrn_orient_matrix_UB_33      -0.00631
_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  0.021
_diffrn_reflns_av_sigmaI/netI    0.051
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            3913
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         60.08
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        -0.79
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.583
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             896.00
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.16
_refine_diff_density_min         -0.13
_refine_ls_extinction_coef       0.269(3)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 gaussian isotropic'
_refine_ls_goodness_of_fit_obs   3.718
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     316
_refine_ls_number_reflns         2677
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0477
_refine_ls_shift/esd_max         1.4670
_refine_ls_shift/esd_mean        0.0400
_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         0.0391
_reflns_number_observed          2677
_reflns_number_total             3650
_reflns_observed_criterion       >3.0sigma(I)
_cod_data_source_file            ja9806534_02.cif
_cod_data_source_block           Compound_1_Racemic_Crystal
_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        2329.1(6)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C13 H13 N3 '
_cod_database_code               4116748