Crystal structure of methyl 1-methyl-3,5-diphenyl-7-tosyl-3,6,7,11b-tetrahydropyrazolo[4',3':5,6]pyrano[3,4-<i>c</i>]quinoline-5a(5<i>H</i>)-carboxylate
Nadendla, Eswar Kumar; Jagadeesan, G.; Kannan, D.; Bakthadoss, Mannickam; Gunasekaran, K.; Acta Crystallographica Section E 70 (2014) o1295–o1296; doi:10.1107/S160053681402515X

data_2240262
_publ_section_title
;
 Crystal structure of methyl
 1-methyl-3,5-diphenyl-7-tosyl-3,6,7,11b-tetrahydropyrazolo[4',3':5,6]pyrano[3,4-<i>c</i>]quinoline-5a(5<i>H</i>)-carboxylate
;
_journal_coeditor_code           SU5015
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1295
_journal_page_last               o1296
_journal_paper_doi               10.1107/S160053681402515X
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C35 H31 N3 O5 S'
_chemical_formula_moiety         'C35 H31 N3 O5 S'
_chemical_formula_sum            'C35 H31 N3 O5 S'
_chemical_formula_weight         605.69
_chemical_name_systematic
'Methyl 1-methyl-3,5-diphenyl-7-tosyl-3,6,7,11b-tetrahydropyrazolo[4',3':5,6]pyrano[3,4-<i>c</i>]quinoline-5a(5<i>H</i>)-carboxylate'
_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                112.708(5)
_cell_angle_beta                 91.908(5)
_cell_angle_gamma                113.180(5)
_cell_formula_units_Z            2
_cell_length_a                   10.781(5)
_cell_length_b                   11.682(5)
_cell_length_c                   14.560(5)
_cell_measurement_reflns_used    8834
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.20
_cell_measurement_theta_min      2.05
_cell_volume                     1517.5(11)
_computing_cell_refinement
;
APEX2 and SAINT (Bruker, 2004)
;
_computing_data_collection
;
APEX2 (Bruker, 2004)
;
_computing_data_reduction
;
SAINT and XPREP (Bruker, 2004)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009) and Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
<i>PLATON</i> (Spek, 2009)
;
_computing_structure_refinement
;
<i>SHELXL97</i> (Sheldrick, 2008)
;
_computing_structure_solution
;
<i>SHELXS97</i> (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       '\w and \f scan'
_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  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23138
_diffrn_reflns_theta_full        26.56
_diffrn_reflns_theta_max         26.56
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.155
_exptl_absorpt_correction_T_max  0.9831
_exptl_absorpt_correction_T_min  0.9790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2004)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.463
_refine_ls_extinction_coef       0.0095(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
<i>SHELXL97</i> (Sheldrick, 2008)
;
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6308
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0517P)^2^+0.4727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1180
_reflns_number_gt                5070
_reflns_number_total             6308
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            su5015sup1.cif
_cod_data_source_block           I
_cod_database_code               2240262
_cod_database_fobs_code          2240262