Dimethyl 11,13-dimethyl-16-[1,2-bis(methoxycarbonyl)ethenyl]-12-oxo-16,17-dioxa-18-azahexacyclo[7.5.1.1^1,4^.1^6,9^.1^10,14^.0^5,15^]octadeca-2,7-diene-2,3-dicarboxylate
Gurbanov, Atash V.; Nikitina, Eugeniya V.; Sorokina, Elena A.; Zubkov, Fedor I.; Khrustalev, Victor N.; Acta Crystallographica Section E 65 (2009) o3243–o3244; doi:10.1107/S1600536809050600

data_2224412
_publ_section_title
;Dimethyl
 11,13-dimethyl-16-[1,2-bis(methoxycarbonyl)ethenyl]-12-oxo-16,17-dioxa-18-azahexacyclo[7.5.1.1^1,4^.1^6,9^.1^10,14^.0^5,15^]octadeca-2,7-diene-2,3-dicarboxylate
;
_journal_coeditor_code           RK2182
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3243
_journal_page_last               o3244
_journal_paper_doi               10.1107/S1600536809050600
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C27 H29 N O11'
_chemical_formula_moiety         'C27 H29 N O11'
_chemical_formula_sum            'C27 H29 N O11'
_chemical_formula_weight         543.51
_chemical_name_systematic
;
Dimethyl
11,13-dimethyl-16-[1,2-bis(methoxycarbonyl)ethenyl]-12-oxo-16,17-dioxa-18-
azahexacyclo[7.5.1.1^1,4^.1^6,9^.1^10,14^.0^5,15^]octadeca-
2,7-diene-2,3-dicarboxylate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.0190(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.1430(7)
_cell_length_b                   9.1365(4)
_cell_length_c                   16.9658(7)
_cell_measurement_reflns_used    5735
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.21
_cell_measurement_theta_min      2.41
_cell_volume                     2492.70(18)
_computing_cell_refinement       '<i>SAINT-Plus</i> (Bruker, 1998)'
_computing_data_collection       '<i>SMART</i> (Bruker, 1998)'
_computing_data_reduction        '<i>SAINT-Plus</i> (Bruker, 1998)'
_computing_molecular_graphics    '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_publication_material  '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXTL</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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    0.0421
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27638
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1998)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.272
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         7186
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0800P)^2^+1.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1334
_refine_ls_wR_factor_ref         0.1505
_reflns_number_gt                5342
_reflns_number_total             7186
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rk2182.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2224412
_cod_database_fobs_code          2224412