Tetramethyl-1-(4-chlorobenzyl)-3a,7a-dihydro-1<i>H</i>-indole-2,3,3a,4-tetracarboxylate
Lee, Chang Kiu; Kang, Youngjin; Jeon, Kiuook; Moon, Suk-Hee; Park, Ki-Min; Acta Crystallographica Section E 63 (2007) o4011–; doi:10.1107/S1600536807042894

data_2215661
_publ_section_title
Tetramethyl-1-(4-chlorobenzyl)-3a,7a-dihydro-1<i>H</i>-indole-2,3,3a,4-tetracarboxylate
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4011
_journal_paper_doi               10.1107/S1600536807042894
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C23 H22 Cl N O8'
_chemical_formula_moiety         'C23 H22 Cl N O8'
_chemical_formula_sum            'C23 H22 Cl N O8'
_chemical_formula_weight         475.87
_chemical_name_systematic
;
Tetramethyl-1-(4-chlorobenzyl)-3a,7a-dihydro-1<i>H</i>-indole-2,3,3a,4-
tetracarboxylate
;
_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           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 112.4710(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8844(8)
_cell_length_b                   12.3350(7)
_cell_length_c                   15.3485(9)
_cell_measurement_reflns_used    6747
_cell_measurement_temperature    446(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.38
_cell_volume                     2254.1(2)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXTL (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      446(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART 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  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13936
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.76
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.219
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.337
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5132
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+0.7066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.1017
_reflns_number_gt                3989
_reflns_number_total             5132
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj2346.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2215661
_cod_database_fobs_code          2215661