Unusual Hetarynic Condensation of 3-Bromo-2-ethoxypyridine with Diisopropyl Ketone Enolate in the Presence of a Complex Base
Ianelli, S.; Nardelli, M.; Belletti, D.; Pasquier, K.; Caubère, P.; Acta Crystallographica Section C 52 (1996) 2097–2100; doi:10.1107/S010827019600501X

data_2005232
_publ_section_title
;
 Unusual Hetarynic Condensation of 3-Bromo-2-ethoxypyridine with
 Diisopropyl Ketone Enolate in the Presence of a Complex Base
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2097
_journal_page_last               2100
_journal_paper_doi               10.1107/S010827019600501X
_journal_volume                  52
_journal_year                    1996
_chemical_formula_analytical     'C21 H28 N2 O3'
_chemical_formula_sum            'C21 H28 N2 O3'
_chemical_formula_weight         356.46
_chemical_name_systematic
;
3,6-diaza-4,5-diethoxy-9,9-dimethyl-10-hydroxy-10-isopropyl-9,10-
dihydroanthracene
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_type_scat_source
'International Tables for Crystallography (1992, Vol. C)'
_cell_angle_alpha                66.59(1)
_cell_angle_beta                 86.91(3)
_cell_angle_gamma                75.93(1)
_cell_formula_units_Z            4
_cell_length_a                   10.580(1)
_cell_length_b                   13.784(3)
_cell_length_c                   15.218(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      8
_cell_volume                     1973.3(6)
_computing_cell_refinement       'LQPARM (Nardelli & Mangia, 1984)'
_computing_data_collection
'local programs (Belletti, Ugozzoli, Cantoni & Pasquinelli, 1979)'
_computing_data_reduction        'local programs'
_computing_molecular_graphics
'ORTEP (Johnson, 1965), ZORTEP (Zsolnai & Pritzkow, 1994)'
_computing_publication_material
'PARST (Nardelli, 1983), PARSTCIF (Nardelli, 1991b)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens-AED three-circle'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6662
_diffrn_reflns_reduction_process standard
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.05
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 50
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.2
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.25
_refine_diff_density_min         -0.24
_refine_ls_extinction_coef       0.0086(4)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.965
_refine_ls_goodness_of_fit_obs   1.524
_refine_ls_hydrogen_treatment    'H atoms riding'
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     484
_refine_ls_number_reflns         6655
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_restrained_S_obs      1.524
_refine_ls_R_factor_obs          0.0527
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0044P)^2^]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1067
_refine_ls_wR_factor_obs         0.0643
_reflns_number_observed          1432
_reflns_number_total             6662
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            cf1097.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               2005232