Crystal structure of 2,3-dimethoxy-5,6,7,8,13,13a-hexahydro-6a,8-diazaindeno[2,1-<i>b</i>]phenanthrene methanol monosolvate
Adizov, Shahobiddin M.; Saidov, Abdusalom Sh.; Turgunov, Kambarali K.; Okmanov, Rasul Ya.; Tashkhodjaev, Bakhodir; Acta Crystallographica Section E 71 (2015) o574–o575; doi:10.1107/S2056989015013286

data_2240922
_publ_section_title
;
 Crystal structure of
 2,3-dimethoxy-5,6,7,8,13,13a-hexahydro-6a,8-diazaindeno[2,1-<i>b</i>]phenanthrene
 methanol monosolvate
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o574
_journal_page_last               o575
_journal_paper_doi               10.1107/S2056989015013286
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C21 H22 N2 O2, C1 H4 O1'
_chemical_formula_moiety         'C21 H22 N2 O2, C1 H4 O1'
_chemical_formula_sum            'C22 H26 N2 O3'
_chemical_formula_weight         366.45
_chemical_melting_point          393(2)
_chemical_name_systematic
;2,3-Dimethoxy-5,6,7,8,13,13a-hexahydro-6a,8-diazaindeno[2,1-<i>b</i>]phenanthrene methanol
monosolvate
;
_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                65.242(4)
_cell_angle_beta                 73.956(4)
_cell_angle_gamma                75.724(4)
_cell_formula_units_Z            2
_cell_length_a                   7.6080(3)
_cell_length_b                   11.8061(5)
_cell_length_c                   12.3327(5)
_cell_measurement_reflns_used    7310
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.6420
_cell_measurement_theta_min      4.0238
_cell_volume                     955.81(8)
_computing_cell_refinement
;
CrysAlis PRO (Oxford Diffraction, 2009)
;
_computing_data_collection
;
CrysAlis PRO (Oxford Diffraction, 2009)
;
_computing_data_reduction
;
CrysAlis PRO (Oxford Diffraction, 2009)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.2576
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19864
_diffrn_reflns_theta_full        75.84
_diffrn_reflns_theta_max         75.84
_diffrn_reflns_theta_min         4.03
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84279
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>CrysAlis PRO</i>; Oxford Diffraction, 2009)
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.171
_refine_diff_density_min         -0.166
_refine_ls_extinction_coef       0.0025(6)
_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   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         3936
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+0.0547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1204
_reflns_number_gt                2889
_reflns_number_total             3936
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            wm5184sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        955.81(7)
_cod_database_code               2240922
_cod_database_fobs_code          2240922