Ethyl 4-(3-chlorophenyl)-3,6-dihydroxy-6-methyl-2-(2-pyridyl)-4,5,6,7-tetrahydroindazole-5-carboxylate
Amirthaganesan, S.; Aridoss, G.; D.Gayathri; Park, Keun Soo; Jeong, Yeon Tae; Acta Crystallographica Section E 66 (2010) o861–; doi:10.1107/S1600536810009360

data_2225596
_publ_section_title
;
 Ethyl
 4-(3-chlorophenyl)-3,6-dihydroxy-6-methyl-2-(2-pyridyl)-4,5,6,7-tetrahydroindazole-5-carboxylate
;
_journal_coeditor_code           NG2744
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o861
_journal_paper_doi               10.1107/S1600536810009360
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C22 H22 Cl N3 O4'
_chemical_formula_moiety         'C22 H22 Cl N3 O4'
_chemical_formula_sum            'C22 H22 Cl N3 O4'
_chemical_formula_weight         427.88
_chemical_name_systematic
;
Ethyl 4-(3-chlorophenyl)-3,6-dihydroxy-6-methyl-2-(2-pyridyl)-4,5,6,7-
tetrahydroindazole-5-carboxylate
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.68(2)
_cell_angle_beta                 90.19(2)
_cell_angle_gamma                115.66(3)
_cell_formula_units_Z            2
_cell_length_a                   8.585(5)
_cell_length_b                   9.053(3)
_cell_length_c                   14.884(3)
_cell_measurement_reflns_used    1965
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.51
_cell_volume                     1038.3(8)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD diffractometer'
_diffrn_measurement_method       '\w and \f scan'
_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  0.0097
_diffrn_reflns_av_sigmaI/netI    0.0128
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4446
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.218
_exptl_absorpt_correction_T_max  0.9576
_exptl_absorpt_correction_T_min  0.9374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.301
_refine_ls_extinction_coef       0.0065(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         3647
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0426P)^2^+0.3338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0923
_reflns_number_gt                3025
_reflns_number_total             3647
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ng2744.cif
_cod_data_source_block           I
_cod_original_cell_volume        1038.3(7)
_cod_database_code               2225596
_cod_database_fobs_code          2225596