4-Desoxy-4β-[(5-methoxy-1<i>H</i>-indol-3-yl)oxalylamino]podophyllotoxin methanol solvate
Feng, Min; Zhao, Ming; Zhang, Jingze; Yang, Zaixin; Chen, Hong; Acta Crystallographica Section E 64 (2008) o2339–; doi:10.1107/S1600536808035319

data_2220067
_publ_section_title
;
 4-Desoxy-4\b-[(5-methoxy-1<i>H</i>-indol-3-yl)oxalylamino]podophyllotoxin
 methanol solvate
;
_journal_coeditor_code           BH2197
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2339
_journal_paper_doi               10.1107/S1600536808035319
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C33 H30 N2 O10, C H4 O'
_chemical_formula_moiety         'C33 H30 N2 O10, C H4 O'
_chemical_formula_sum            'C34 H34 N2 O11'
_chemical_formula_weight         646.63
_chemical_name_systematic
;
4-Desoxy-4\b-[(5-methoxy-1H-indol-3-yl)oxalylamino]podophyllotoxin
methanol solvate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.58(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.228(2)
_cell_length_b                   9.8360(16)
_cell_length_c                   26.667(5)
_cell_measurement_reflns_used    8161
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.4565
_cell_measurement_theta_min      1.6731
_cell_volume                     3192.2(10)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC, 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn CCD area-detector'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            22853
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  0.9879
_exptl_absorpt_correction_T_min  0.9761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku/MSC, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.271
_refine_ls_extinction_coef       0.0201(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     893
_refine_ls_number_reflns         7730
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0825P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1265
_reflns_number_gt                6754
_reflns_number_total             7730
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bh2197.cif
_cod_data_source_block           I
_cod_original_cell_volume        3192.2(9)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2220067
_cod_database_fobs_code          2220067