Ethyl 4-(2,3,5,6-tetrahydro-3,3-dimethyl-5,6-dioxo-1,2-cycloheptapyrazol-2-yl)benzoate
Kubo, Kanji; Mori, Akira; Acta Crystallographica Section E 57 (2001) o328–o329; doi:10.1107/S1600536801004445

data_2200163
_publ_section_title
;Ethyl
 4-(2,3,5,6-tetrahydro-3,3-dimethyl-5,6-dioxo-1,2-cycloheptapyrazol-2-yl)benzoate
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o328
_journal_page_last               o329
_journal_paper_doi               10.1107/S1600536801004445
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          'C19 H18 N2 O4'
_chemical_formula_moiety         'C19 H18 N2 O4'
_chemical_formula_sum            'C19 H18 N2 O4'
_chemical_formula_weight         338.35
_chemical_name_systematic
;
Ethyl
4-(2,3,5,6-tetrahydro-3,3-dimethyl-5,6-dioxo-1,2-cycloheptapyrazol-2-yl)-
benzoate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.028(3)
_cell_length_b                   19.166(3)
_cell_length_c                   9.4466(5)
_cell_measurement_reflns_used    16
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.9
_cell_measurement_theta_min      9.2
_cell_volume                     3445.1(8)
_computing_cell_refinement       ' CAD-4 Software'
_computing_data_collection       ' CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        ' MolEN (Fair, 1990)'
_computing_molecular_graphics    'Xtal_GX (Hall & du Boulay, 1995)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    ' SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full .000
_diffrn_measured_fraction_theta_max .999
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0000
_diffrn_reflns_av_sigmaI/netI    .2271
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4149
_diffrn_reflns_theta_full        28.0
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        .5
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .093
_exptl_absorpt_correction_T_max  .9980
_exptl_absorpt_correction_T_min  .9691
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   ' (North et al., 1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          .33
_exptl_crystal_size_mid          .27
_exptl_crystal_size_min          .13
_refine_diff_density_max         .204
_refine_diff_density_min         -.242
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   .890
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      .890
_refine_ls_R_factor_all          .2850
_refine_ls_R_factor_gt           .0544
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0539P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1581
_reflns_number_gt                1280
_reflns_number_total             4149
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv6009.cif
_cod_data_source_block           I
_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_original_cell_volume        3445.1(7)
_cod_database_code               2200163
_cod_database_fobs_code          2200163