15-(4-Chlorophenyl)-6b-hydroxy-17-methyl-6b,7,16,17-tetrahydro-7,14a-methanonaphtho[1',8':1,2,3]pyrrolo[3',2':8,8a]azuleno[5,6-<i>b</i>]quinolin-14(15<i>H</i>)-one methanol hemisolvate
Joseph, J. M.; Viswanathan, Vijayan; Velmurugan, Devadasan; IUCrData 1 (2016) x160637–; doi:10.1107/S2414314616006374

data_1543232
_publ_section_title
;
 15-(4-Chlorophenyl)-6b-hydroxy-17-methyl-6b,7,16,17-tetrahydro-7,14a-methanonaphtho[1',8':1,2,3]pyrrolo[3',2':8,8a]azuleno[5,6-<i>b</i>]quinolin-14(15<i>H</i>)-one
 methanol hemisolvate
;
_journal_coeditor_code           SU4031
_journal_issue                   4
_journal_name_full               IUCrData
_journal_page_first              x160637
_journal_paper_doi               10.1107/S2414314616006374
_journal_volume                  1
_journal_year                    2016
_chemical_formula_iupac          'C34 H25 Cl N2 O2, 0.5C H4 O'
_chemical_formula_moiety         'C34 H25 Cl N2 O2, 0.5(C H4 O)'
_chemical_formula_sum            'C34.5 H26.5 Cl N2 O2.5'
_chemical_formula_weight         544.53
_chemical_name_common
'2-(4-Chlorophenyl)-15-hydroxy-4-methyl-4,18-diazaoctacyclo[14.11.1.1^6,10^.0^1,5^.0^5,15^.0^17,26^.0^19,24^.0^14,29^]nonacosa-6,8,10(29),11,13,17,19(24),20,22,25-decaen-27-one methanol hemisolvate'
_chemical_name_systematic
;15-(4-Chlorophenyl)-6b-hydroxy-17-methyl-6b,7,16,17-tetrahydro-
7,14a-methanonaphtho[1',8':1,2,3]pyrrolo[3',2':8,8a]azuleno[5,6-<i>b</i>]quinolin-14(15<i>H</i>)-one methanol hemisolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                69.3940(10)
_cell_angle_beta                 72.3880(10)
_cell_angle_gamma                70.8710(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3848(3)
_cell_length_b                   10.4306(3)
_cell_length_c                   14.4513(4)
_cell_measurement_reflns_used    5568
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.54
_cell_measurement_theta_min      1.54
_cell_volume                     1352.92(7)
_computing_cell_refinement
;
SAINT (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART APEXII area-detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20173
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.543
_diffrn_reflns_theta_min         1.540
_exptl_absorpt_coefficient_mu    0.179
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       block
_exptl_crystal_F_000             569
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.440
_refine_ls_extinction_coef       0.019(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         5563
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1116P)^2^+0.2946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1644
_refine_ls_wR_factor_ref         0.1781
_reflns_number_gt                4425
_reflns_number_total             5563
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su4031sup1.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C34.50 H26.50 Cl N2 O2.50'
_cod_database_code               1543232
_cod_database_fobs_code          1543232
_shelx_hkl_checksum              93403
_shelx_res_checksum              65064
_shelxl_version_number           2014/6