Ethyl 3,6-dihydroxy-6-methyl-4-phenyl-4,5,6,7-tetrahydro-1<i>H</i>-indazole-5-carboxylate monohydrate
Maharramov, Abel M.; Ismiyev, Arif I.; Rashidov, Bahruz A.; Acta Crystallographica Section E 67 (2011) o480–; doi:10.1107/S160053681100242X

data_2229193
_publ_section_title
;
 Ethyl
 3,6-dihydroxy-6-methyl-4-phenyl-4,5,6,7-tetrahydro-1<i>H</i>-indazole-5-carboxylate
 monohydrate
;
_journal_coeditor_code           PV2374
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o480
_journal_paper_doi               10.1107/S160053681100242X
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C17 H20 N2 O4, H2 O'
_chemical_formula_moiety         'C17 H20 N2 O4, H2 O'
_chemical_formula_sum            'C17 H22 N2 O5'
_chemical_formula_weight         334.37
_chemical_name_systematic
;
Ethyl 3,6-dihydroxy-6-methyl-4-phenyl-4,5,6,7-tetrahydro-1<i>H</i>-indazole-5-
carboxylate monohydrate
;
_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                99.363(6)
_cell_angle_beta                 95.281(6)
_cell_angle_gamma                112.271(4)
_cell_formula_units_Z            2
_cell_length_a                   6.9964(15)
_cell_length_b                   8.8647(19)
_cell_length_c                   15.124(4)
_cell_measurement_reflns_used    909
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.58
_cell_measurement_theta_min      2.54
_cell_volume                     844.2(3)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w'
_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  0.0652
_diffrn_reflns_av_sigmaI/netI    0.1183
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6332
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_T_max  0.9808
_exptl_absorpt_correction_T_min  0.9808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.369
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         2889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0768
_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^)+(0.0611P)^2^+0.4352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1863
_refine_ls_wR_factor_ref         0.1980
_reflns_number_gt                2327
_reflns_number_total             2889
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pv2374.cif
_cod_data_source_block           I
_cod_database_code               2229193
_cod_database_fobs_code          2229193