Diethyl 2,6-dihydroxy-4-(3-nitrophenyl)-2,6-bis(trifluoromethyl)piperidine-3,5-dicarboxylate
Fun, Hoong-Kun; Arshad, Suhana; Reddy, B. Palakshi; Vijayakumar, V.; Sarveswari, S.; Acta Crystallographica Section E 68 (2012) o400–o401; doi:10.1107/S1600536811055346

data_2233618
_publ_section_title
;
 Diethyl
 2,6-dihydroxy-4-(3-nitrophenyl)-2,6-bis(trifluoromethyl)piperidine-3,5-dicarboxylate
;
_journal_coeditor_code           RZ2690
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o400
_journal_page_last               o401
_journal_paper_doi               10.1107/S1600536811055346
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C19 H20 F6 N2 O8'
_chemical_formula_moiety         'C19 H20 F6 N2 O8'
_chemical_formula_sum            'C19 H20 F6 N2 O8'
_chemical_formula_weight         518.37
_chemical_name_systematic
;
Diethyl 2,6-dihydroxy-4-(3-nitrophenyl)-
2,6-bis(trifluoromethyl)piperidine-3,5-dicarboxylate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 91.049(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.7353(16)
_cell_length_b                   15.2025(14)
_cell_length_c                   17.3003(16)
_cell_measurement_reflns_used    4307
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      2.93
_cell_volume                     4663.7(7)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
;
Bruker SMART APEXII DUO CCD area-detector
;
_diffrn_measurement_method       '\f and \w scans'
_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  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19801
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.76
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_T_max  0.9804
_exptl_absorpt_correction_T_min  0.9701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.188
_refine_ls_extinction_coef       0.00084(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXTL (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         5339
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0493P)^2^+2.0652P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1247
_reflns_number_gt                3229
_reflns_number_total             5339
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz2690.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2233618
_cod_database_fobs_code          2233618