Molecular structure of 5,6-bis(dimethylamino)acenaphthene, 5,6-bis(dimethylamino)acenaphthylene, and their monohydrobromides: a comparison with some naphthalene proton sponges
Pozharskii, Alexander F.; Ozeryanskii, Valery A.; Starikova, Zoya A.; Journal of the Chemical Society, Perkin Transactions 2  (2002) 318–; doi:10.1039/b106725g

data_7204984
_publ_section_title
;
 Molecular structure of 5,6-bis(dimethylamino)acenaphthene,
 5,6-bis(dimethylamino)acenaphthylene, and their monohydrobromides: a
 comparison with some naphthalene proton sponges
;
_journal_issue                   2
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              318
_journal_paper_doi               10.1039/b106725g
_journal_year                    2002
_chemical_formula_sum            'C16 H20 N2'
_chemical_formula_weight         240.34
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 111.94(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.183(3)
_cell_length_b                   8.656(2)
_cell_length_c                   11.822(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      9
_cell_volume                     1441.2(6)
_computing_cell_refinement       'CAD4 Enraf-Nonius'
_computing_data_collection       'CAD4 Enraf-Nonius'
_computing_data_reduction        'SHELXTL PLUS 5'
_computing_molecular_graphics    'SHELXTL PLUS 5'
_computing_publication_material  'SHELXTL PLUS 5'
_computing_structure_refinement  'SHELXTL PLUS 5'
_computing_structure_solution    'SHELXTL PLUS 5'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'CAD4 Enraf-Nonius'
_diffrn_measurement_method       'q\5/3q scans'
_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  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0594
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3418
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         1.45
_diffrn_standards_decay_%        2.5
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_description       needle
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.021
_refine_ls_goodness_of_fit_obs   1.272
_refine_ls_hydrogen_treatment    'rogid mode'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         3090
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_restrained_S_obs      1.272
_refine_ls_R_factor_all          0.2224
_refine_ls_R_factor_obs          0.0771
_refine_ls_shift/esd_max         -0.015
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1319P)^2^+0.3319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3367
_refine_ls_wR_factor_obs         0.2161
_reflns_number_observed          1045
_reflns_number_total             3137
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b106725g.txt
_cod_data_source_block           p
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1319P)^2^+0.3319P] where P=(Fo^2^+2Fc^2^)/3' 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^)+(0.1319P)^2^+0.3319P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1441.2(5)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7204984