5-Carboxylato-5-hydroxy-4-(4-methoxybenzoyl)-3-(4-methoxyphenyl)-1,1-dimethyl-4,5-dihydro-1<i>H</i>-pyrazol-1-ium monohydrate
Demir, Sibel; Dinçer, Muharrem; Yıldırım, İsmail; Kayademir, Aslıhan; Acta Crystallographica Section E 61 (2005) o3540–o3542; doi:10.1107/S1600536805031053

data_2207282
_publ_section_title
;5-Carboxylato-5-hydroxy-4-(4-methoxybenzoyl)-3-(4-methoxyphenyl)-1,1-dimethyl-4,5-dihydro-1<i>H</i>-pyrazol-1-ium
 monohydrate
;
_journal_coeditor_code           LH6478
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3540
_journal_page_last               o3542
_journal_paper_doi               10.1107/S1600536805031053
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C21 H22 N2 O6, H2 O'
_chemical_formula_moiety         'C21 H22 N2 O6, H2 O'
_chemical_formula_sum            'C21 H24 N2 O7'
_chemical_formula_weight         416.42
_chemical_name_systematic
;5-carboxylato-5-hydroxy-4-(4-methoxybenzoyl)-3-(4-methoxyphenyl)-1,1-dimethyl-
4,5-dihydro-1H-pyrazol-1-ium
 monohydrate
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.896(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.5325(8)
_cell_length_b                   16.0283(11)
_cell_length_c                   7.8717(4)
_cell_measurement_reflns_used    18802
_cell_measurement_temperature    296
_cell_measurement_theta_max      28.04
_cell_measurement_theta_min      1.77
_cell_volume                     2078.3(2)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED32 (Stoe & Cie, 2002)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material
'WinGX (Farrugia, 1999) and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS-2'
_diffrn_measurement_method       'rotation method'
_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  0.0589
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            19824
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   '(X-RED; Stoe & Cie, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.331
_refine_ls_extinction_coef       0.0073(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4084
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0745P)^2^+0.0106P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1303
_reflns_number_gt                2753
_reflns_number_total             4084
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6478.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2207282
_cod_database_fobs_code          2207282