Crystal strucutre of <i>rac</i>-methyl (11a<i>R</i>*,12<i>S</i>*,13<i>R</i>*,15a<i>S</i>*,15b<i>S</i>*)-11-oxo-11,11a,12,13-tetrahydro-9<i>H</i>,15b<i>H</i>-13,15a-epoxyisoindolo[1,2-<i>c</i>]pyrrolo[1,2-<i>a</i>][1,4]benzodiazepine-12-carboxylate
Zaytsev, Vladimir P.; Orlova, Daria N.; Gurbanov, Atash V.; Zubkov, Fedor I.; Khrustalev, Victor N.; Acta Crystallographica Section E 70 (2014) o1225–o1226; doi:10.1107/S1600536814023344

data_2240167
_publ_section_title
;
 Crystal strucutre of <i>rac</i>-methyl
 (11a<i>R</i>*,12<i>S</i>*,13<i>R</i>*,15a<i>S</i>*,15b<i>S</i>*)-11-oxo-11,11a,12,13-tetrahydro-9<i>H</i>,15b<i>H</i>-13,15a-epoxyisoindolo[1,2-<i>c</i>]pyrrolo[1,2-<i>a</i>][1,4]benzodiazepine-12-carboxylate
;
_journal_coeditor_code           LD2132
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1225
_journal_page_last               o1226
_journal_paper_doi               10.1107/S1600536814023344
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C21 H18 N2 O4'
_chemical_formula_moiety         'C21 H18 N2 O4'
_chemical_formula_sum            'C21 H18 N2 O4'
_chemical_formula_weight         362.37
_chemical_name_systematic
;<i>rac</i>-Methyl
(11a<i>R</i>*,12<i>S</i>*,13<i>R</i>*,15a<i>S</i>*,15b<i>S</i>*)-11-oxo-11,11a,12,13-tetrahydro-9<i>H</i>,15b<i>H</i>-13,15a-epoxyisoindolo[1,2-<i>c</i>]pyrrolo[1,2-<i>a</i>][1,4]benzodiazepine-12-carboxylate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 98.2100(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.1565(3)
_cell_length_b                   14.2567(5)
_cell_length_c                   14.6664(5)
_cell_measurement_reflns_used    8798
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.57
_cell_measurement_theta_min      2.52
_cell_volume                     1688.00(10)
_computing_cell_refinement
;
SAINT (Bruker, 2001)
;
_computing_data_collection
;
APEX2 (Bruker, 2005)
;
_computing_data_reduction
;
SAINT (Bruker, 2001)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXTL (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX DUO 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  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25733
_diffrn_reflns_theta_full        32.60
_diffrn_reflns_theta_max         32.60
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2003)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.265
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         6162
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0646P)^2^+0.565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1188
_reflns_number_gt                5097
_reflns_number_total             6162
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ld2132sup1.cf
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2240167
_cod_database_fobs_code          2240167