<i>rac</i>-(<i>Z</i>)-Methyl 1-benzyl-3-[(3-hydroxyquinuclidin-2-ylidene)methyl]-1<i>H</i>-indole-6-carboxylate
Penthala, Narsimha Reddy; Ponugoti, Purushotham Rao; Parkin, Sean; Crooks, Peter A.; Acta Crystallographica Section E 68 (2012) o3111–; doi:10.1107/S1600536812040731

data_2236312
_publ_section_title
;
 <i>rac</i>-(<i>Z</i>)-Methyl
 1-benzyl-3-[(3-hydroxyquinuclidin-2-ylidene)methyl]-1<i>H</i>-indole-6-carboxylate
;
_journal_coeditor_code           HG5242
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3111
_journal_paper_doi               10.1107/S1600536812040731
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C25 H26 N2 O3'
_chemical_formula_moiety         'C25 H26 N2 O3'
_chemical_formula_sum            'C25 H26 N2 O3'
_chemical_formula_weight         402.48
_chemical_name_systematic
;
<i>rac</i>-(<i>Z</i>)-Methyl
1-benzyl-3-[(3-hydroxyquinuclidin-2-ylidene)methyl]-1<i>H</i>-indole-6-
carboxylate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.6705(7)
_cell_angle_beta                 80.0939(7)
_cell_angle_gamma                85.9410(7)
_cell_formula_units_Z            2
_cell_length_a                   6.16190(10)
_cell_length_b                   10.3119(2)
_cell_length_c                   16.5959(3)
_cell_measurement_reflns_used    4571
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1006.04(3)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and local procedures
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 9.1
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\w scans at fixed \c = 55\%'
_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  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9126
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.04
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.197
_refine_ls_extinction_coef       0.023(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         4597
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0442P)^2^+0.3522P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1023
_reflns_number_gt                3831
_reflns_number_total             4597
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            hg5242.cif
_cod_data_source_block           I
_cod_database_code               2236312
_cod_database_fobs_code          2236312