Paraherquamide E
Aree, Thammarat; Antia, Bassey S.; Ekpa, Okon D.; Kittakoop, Prasat; Acta Crystallographica Section E 66 (2010) o2227–; doi:10.1107/S1600536810030795

data_2227311
_publ_section_title
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 Paraherquamide E
;
_journal_coeditor_code           CI5149
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2227
_journal_paper_doi               10.1107/S1600536810030795
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C28 H35 N3 O4'
_chemical_formula_moiety         'C28 H35 N3 O4'
_chemical_formula_sum            'C28 H35 N3 O4'
_chemical_formula_weight         477.59
_chemical_melting_point          ?
_chemical_name_common
;
(1'<i>R</i>,5'a<i>S</i>,7'<i>R</i>,8'a<i>S</i>,9'a<i>R</i>)-2',3',8'a,9'-
tetrahydro-1'-hydroxy-1',4,4,8',8',11'-hexamethyl-14-
deoxyspiro[4<i>H</i>,8<i>H</i>-1,4-dioxepino[2,3-<i>g</i>]indole-
8,7'(8'<i>H</i>)-[5<i>H</i>,6<i>H</i>-
5a,9a](iminomethano)[1<i>H</i>]cyclopent[<i>f</i>]indolizine]-
9,10'(10<i>H</i>)-dione
;
_chemical_name_systematic        'Paraherquamide E'
_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                   6.5069(2)
_cell_length_b                   16.0351(8)
_cell_length_c                   23.9713(11)
_cell_measurement_reflns_used    1372
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      19.70
_cell_measurement_theta_min      2.54
_cell_volume                     2501.14(19)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'Mercury (Macrae <i>et al.</i> 2006)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.824
_diffrn_measurement_device_type  'Bruker SMART APEXII 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  0.0493
_diffrn_reflns_av_sigmaI/netI    0.0732
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            8444
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.18
_diffrn_reflns_theta_min         1.53
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.9543
_exptl_absorpt_correction_T_min  0.9457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.157
_refine_diff_density_min         -0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         2889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0463P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.1022
_reflns_number_gt                1746
_reflns_number_total             2889
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci5149.cif
_cod_data_source_block           I
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
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_cod_database_code               2227311
_cod_database_fobs_code          2227311