An orthorhombic polymorph of a cyclization product of perindopril
Bojarska, Joanna; Maniukiewicz, Waldemar; Sieroń, Lesław; Remko, Milan; Acta Crystallographica Section C 69 (2013) 630–633; doi:10.1107/S0108270113011025

data_2019004
_publ_section_title
;
 An orthorhombic polymorph of a cyclization product of perindopril
;
_journal_coeditor_code           TP3019
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              630
_journal_page_last               633
_journal_paper_doi               10.1107/S0108270113011025
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C19 H30 N2 O4'
_chemical_formula_moiety         'C19 H30 N2 O4'
_chemical_formula_sum            'C19 H30 N2 O4'
_chemical_formula_weight         350.45
_chemical_name_systematic
'Ethyl (2<i>S</i>)-2-[(3<i>S</i>,5a<i>S</i>,9a<i>S</i>,10a<i>S</i>)-3-methyl-1,4-dioxo-5a,6,7,8,9,9a,10,10a-octahydro-3<i>H</i>-pyrazino[1,2-<i>a</i>]indol-2-yl]pentanoate'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.2089(10)
_cell_length_b                   17.9875(17)
_cell_length_c                   23.697(2)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.73
_cell_measurement_theta_min      3.08
_cell_volume                     3925.3(7)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2008)'
_computing_molecular_graphics
'PLATON (Spek, 2009) and Mercury (Macrae <i>et al.</i>, 2008)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         '30W microsource with MonoCap capillary'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            39028
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        66.00
_diffrn_reflns_theta_max         66.00
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.371
_refine_ls_abs_structure_details 'Flack (1983), 2958 Friedel pairs'
_refine_ls_abs_structure_Flack   0.1(3)
_refine_ls_extinction_coef       0.00149(10)
_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   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         6791
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0567
_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^)+(0.04P)^2^+4.25P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1281
_refine_ls_wR_factor_ref         0.1445
_reflns_number_gt                5706
_reflns_number_total             6791
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tp3019.cif
_cod_data_source_block           Io
_cod_database_code               2019004
_cod_database_fobs_code          2019004