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_7204987
_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            'C18 H22 Br N3'
_chemical_formula_weight         360.30
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 94.721(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.400(2)
_cell_length_b                   11.7675(10)
_cell_length_c                   10.6404(9)
_cell_measurement_temperature    200(2)
_cell_volume                     3543.9(5)
_computing_cell_refinement       'SMART Bruker'
_computing_data_collection       'SMART Bruker'
_computing_data_reduction        'SMART Bruker'
_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      200(2)
_diffrn_measurement_device       'SMART Bruker'
_diffrn_measurement_method       'phi and omega 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  0.0801
_diffrn_reflns_av_sigmaI/netI    0.1610
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18363
_diffrn_reflns_theta_max         30.07
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    2.320
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7143
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            light-brown
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       needle
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.655
_refine_ls_goodness_of_fit_obs   0.914
_refine_ls_hydrogen_treatment    isotropic
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         5103
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.804
_refine_ls_restrained_S_obs      0.914
_refine_ls_R_factor_all          0.1283
_refine_ls_R_factor_obs          0.0368
_refine_ls_shift/esd_max         -0.022
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0179P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0700
_refine_ls_wR_factor_obs         0.0498
_reflns_number_observed          1999
_reflns_number_total             5145
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b106725g.txt
_cod_data_source_block           zam
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0179P)^2^+0.0000P] 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^)+(0.0179P)^2^+0.0000P] 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        3544.0(5)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7204987