Methyl 2-benzyl-1-benzyloxy-6a-methyl-1,2,3,3a,4,6a-hexahydrocyclopenta[<i>b</i>]pyrrole-3a-carboxylate: hydrogen-bonded <i>R</i>~<b>4~</b>^<b>4^</b>(24) sheets
Low, John Nicolson; Cobo, Justo; Nogueras, Manuel; Loaiza, Alix Elena; Jaramillo-Gómez, Luz Marina; Acta Crystallographica Section E 62 (2006) o165–o167; doi:10.1107/S1600536805040742

data_2207834
_publ_section_title
;Methyl
 2-benzyl-1-benzyloxy-6a-methyl-1,2,3,3a,4,6a-hexahydrocyclopenta[<i>b</i>]pyrrole-3a-carboxylate:
 hydrogen-bonded <i>R</i>~<b>4~</b>^<b>4^</b>(24) sheets
;
_journal_coeditor_code           LH6566
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o165
_journal_page_last               o167
_journal_paper_doi               10.1107/S1600536805040742
_journal_volume                  62
_journal_year                    2006
_chemical_formula_moiety         'C24 H27 N O3'
_chemical_formula_sum            'C24 H27 N O3'
_chemical_formula_weight         377.47
_chemical_melting_point          355
_chemical_name_systematic
;
Methyl 2-benzyl-1-benzyloxy-6a-methyl-1,2,3,3a,4,6a-hexahydro-
1-azapentalene-3a-carboxylate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.8410(17)
_cell_length_b                   20.584(4)
_cell_length_c                   22.344(2)
_cell_measurement_reflns_used    4921
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.50
_cell_measurement_theta_min      6.44
_cell_volume                     4066.2(12)
_computing_cell_refinement       'DIRAX/LSQ (Duisenberg et al., 2000)'
_computing_data_collection       'COLLECT (Hooft, 2004)'
_computing_data_reduction        'EvalCCD (Duisenberg et al., 2003)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material
'SHELXL97 and WordPerfect macro PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement
'OSCAIL (McArdle, 2003 and SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Bruker--Nonius KappaCCD'
_diffrn_measurement_method       \f--\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            48795
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         6.44
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.9904
_exptl_absorpt_correction_T_min  0.9700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'[SADABS (Sheldrick, 2003) and EvalCCD (Duisenberg et al., 2003)]'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4921
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0174P)^2^+3.2146P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.1085
_reflns_number_gt                3477
_reflns_number_total             4921
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6566.cif
_cod_data_source_block           I
_cod_database_code               2207834
_cod_database_fobs_code          2207834