<i>tert</i>-Butyl <i>N</i>-[(11-<i>exo</i>-benzyloxycarbonyl-8-oxopentacyclo[5.4.0.0^2,6^.0^3,10^.0^5,9^]undecane-11-<i>endo</i>-yloxy)carbonylmethyl]carbamate
Karpoormath, Rajshekhar; Govender, Thavendran; Govender, Patrick; Kruger, Hendrik G.; Maguire, Glenn E. M.; Acta Crystallographica Section E 66 (2010) o2607–o2608; doi:10.1107/S1600536810036627

data_2227871
_publ_section_title
;
 <i>tert</i>-Butyl
 <i>N</i>-[(11-<i>exo</i>-benzyloxycarbonyl-8-oxopentacyclo[5.4.0.0^2,6^.0^3,10^.0^5,9^]undecane-11-<i>endo</i>-yloxy)carbonylmethyl]carbamate
;
_journal_coeditor_code           OM2360
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2607
_journal_page_last               o2608
_journal_paper_doi               10.1107/S1600536810036627
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C26 H29 N O7'
_chemical_formula_moiety         'C26 H29 N O7'
_chemical_formula_sum            'C26 H29 N O7'
_chemical_formula_weight         467.50
_chemical_name_systematic
;
<i>tert</i>-Butyl <i>N</i>-[(11-<i>exo</i>-benzyloxycarbonyl-8-
oxopentacyclo[5.4.0.0^2,6^.0^3,10^.0^5,9^]undecane-11-<i>endo</i>-
yloxy)carbonylmethyl]carbamate
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 107.6790(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7260(2)
_cell_length_b                   27.5398(7)
_cell_length_c                   9.3500(2)
_cell_measurement_reflns_used    8919
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.13
_cell_measurement_theta_min      5.92
_cell_volume                     2386.14(9)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker Kappa DUO APEXII'
_diffrn_measurement_method       '0.5\% \f scans and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8919
_diffrn_reflns_theta_full        68.13
_diffrn_reflns_theta_max         68.13
_diffrn_reflns_theta_min         5.92
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.6943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.178
_refine_ls_abs_structure_details 'Flack (1983), 1760 Friedel pairs'
_refine_ls_abs_structure_Flack   0.00(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         3948
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0509P)^2^+1.0452P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.0999
_reflns_number_gt                3802
_reflns_number_total             3948
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om2360.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2227871
_cod_database_fobs_code          2227871