Solution and solid state structure and tautomerism of azo coupled enaminone derivatives of benzoylacetone.
Sim°unek, Petr; Bertolasi, Valerio; Pesková, Markéta; Machácek, Vladimír; Lycka, Antonín; Organic & biomolecular chemistry 3 (2005) 1217–1226; doi:10.1039/b500173k

data_7150063
_publ_section_title
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 Solution and solid state structure and tautomerism of azo coupled
 enaminone derivatives of benzoylacetone.
;
_journal_issue                   7
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              1217
_journal_page_last               1226
_journal_paper_doi               10.1039/b500173k
_journal_volume                  3
_journal_year                    2005
_chemical_formula_moiety         'C22 H18 Br N3 O'
_chemical_formula_sum            'C22 H18 Br N3 O'
_chemical_formula_weight         420.30
_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_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.075(1)
_cell_angle_beta                 88.902(2)
_cell_angle_gamma                81.541(1)
_cell_formula_units_Z            2
_cell_length_a                   9.3969(3)
_cell_length_b                   10.5034(3)
_cell_length_c                   10.5516(4)
_cell_measurement_reflns_used    19612
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      3.4
_cell_volume                     973.97(6)
_computing_cell_refinement       'Denzo SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997)'
_computing_data_reduction        'Denzo SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP III (Burnett & Johnson, 1996)'
_computing_publication_material
;
SHELXL-97 (Sheldrick, 1997), Nardelli (PARST, 1995)'
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '\f scans and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12849
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.0
_diffrn_reflns_theta_min         3.4
_exptl_absorpt_coefficient_mu    2.126
_exptl_absorpt_correction_T_max  0.813
_exptl_absorpt_correction_T_min  0.700
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SORTAV (R.H. Blessing, Acta Crystallogr., 1995, A51, 33)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5579
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+0.4868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0850
_reflns_number_gt                5075
_reflns_number_total             5579
_reflns_threshold_expression     'I >2sigma(I)'
_cod_data_source_file            b500173k.txt
_cod_data_source_block           (I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               7150063