Crystal structure of 4-(6-bromo-4-oxo-4<i>H</i>-chromen-3-yl)-2-methylamino-3-nitropyrano[3,2-<i>c</i>]chromen-5(4<i>H</i>)-one chloroform monosolvate
Raja, Rajamani; Kandhasamy, Subramani; Perumal, Paramasivam T.; SubbiahPandi, A.; Acta Crystallographica Section E 71 (2015) o648–o649; doi:10.1107/S2056989015014553

data_2241007
_publ_section_title
;
 Crystal structure of
 4-(6-bromo-4-oxo-4<i>H</i>-chromen-3-yl)-2-methylamino-3-nitropyrano[3,2-<i>c</i>]chromen-5(4<i>H</i>)-one
 chloroform monosolvate
;
_journal_coeditor_code           HB7473
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o648
_journal_page_last               o649
_journal_paper_doi               10.1107/S2056989015014553
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C22 H13 Br N2 O7, C H Cl3 '
_chemical_formula_moiety         'C22 H13 Br N2 O7, C H Cl3 '
_chemical_formula_sum            'C23 H14 Br Cl3 N2 O7'
_chemical_formula_weight         616.62
_chemical_name_systematic
'4-(6-Bromo-4-oxo-4<i>H</i>-chromen-3-yl)-2-methylamino-3-nitropyrano[3,2-<i>c</i>]chromen-5(4<i>H</i>)-one chloroform 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                80.8040(10)
_cell_angle_beta                 68.4220(10)
_cell_angle_gamma                70.7350(10)
_cell_formula_units_Z            2
_cell_length_a                   9.8816(2)
_cell_length_b                   11.9237(3)
_cell_length_c                   12.0616(3)
_cell_measurement_reflns_used    3672
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.82
_cell_volume                     1246.36(5)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2008)
;
_computing_data_collection
;
<i>APEX2</i> (Bruker, 2008)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2008)
;
_computing_molecular_graphics
;
<i>ORTEP-3 for Windows</i> (Farrugia, 2012)
;
_computing_publication_material
;
<i>SHELXL97</i>  (Sheldrick, 2008) and <i>PLATON</i> (Spek,
2009)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       '\w and \f 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  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17277
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    2.018
_exptl_absorpt_correction_T_max  0.6324
_exptl_absorpt_correction_T_min  0.5386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2008)
;
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       colourless
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.528
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         4389
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.251
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0626P)^2^+1.1978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1196
_reflns_number_gt                3672
_reflns_number_total             4389
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb7473sup1.cif
_cod_data_source_block           I
_cod_database_code               2241007
_cod_database_fobs_code          2241007