Kallolide A acetate pyrazoline
Rodríguez-Escudero, Idaliz; Marrero, Jeffrey; Rodríguez, Abimael D.; Acta Crystallographica Section E 68 (2012) o41–o42; doi:10.1107/S1600536811051890

data_2233317
_publ_section_title
;
 Kallolide A acetate pyrazoline
;
_journal_coeditor_code           WN2456
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o41
_journal_page_last               o42
_journal_paper_doi               10.1107/S1600536811051890
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C23 H28 N2 O5'
_chemical_formula_moiety         'C23 H28 N2 O5'
_chemical_formula_sum            'C23 H28 N2 O5'
_chemical_formula_weight         412.47
_chemical_name_common            'kallolide A acetate pyrazoline'
_chemical_name_systematic
;
7-methyl-16-oxo-4,10-bis(prop-1-en-2-yl)-17,18-dioxa-14,15-
diazatetracyclo[9.4.2.1^6,9^.0^1,12^]octadeca-6,8,14-trien-5-yl acetate
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.593(6)
_cell_length_b                   12.426(7)
_cell_length_c                   17.099(10)
_cell_measurement_reflns_used    9306
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.71
_cell_measurement_theta_min      2.26
_cell_volume                     2251(2)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 1999)'
_computing_data_collection       '<i>SMART-NT</i> (Bruker, 1998)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 1999)'
_computing_molecular_graphics    '<i>SHELXTL</i> (Sheldrick, 2008<i>b</i>)'
_computing_publication_material  '<i>SHELXTL</i> (Sheldrick, 2008<i>b</i>)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008<i>b</i>)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008<i>b</i>)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker SMART 1K CCD'
_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  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0277
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14038
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.9915
_exptl_absorpt_correction_T_min  0.9664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008<i>a</i>)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.225
_refine_ls_extinction_coef       0.061(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     '<i>SHELXL97</i> (Sheldrick, 2008a)'
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         2583
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0552P)^2^+0.3145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1182
_reflns_number_gt                2160
_reflns_number_total             2583
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            wn2456.cif
_cod_data_source_block           I
_cod_database_code               2233317
_cod_database_fobs_code          2233317