An orthorhombic polymorph of palonosetron hydrochloride
Krishnan Ravikumar; Balasubramanian Sridhar; Acta Crystallographica Section E 63 (2007) o1404–o1406; doi:10.1107/S1600536807007829

data_2212555
_publ_section_title
;
 An orthorhombic polymorph of palonosetron hydrochloride
;
_journal_coeditor_code           GK2050
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1404
_journal_page_last               o1406
_journal_paper_doi               10.1107/S1600536807007829
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C19 H25 O N2 + , Cl -'
_chemical_formula_moiety         'C19 H25 O N2 + , Cl -'
_chemical_formula_sum            'C19 H25 Cl N2 O'
_chemical_formula_weight         332.86
_chemical_name_common            'Palonosetron hydrochloride'
_chemical_name_systematic
;
2-[(S)-1-azoniabicyclo[2.2.2]oct-3-yl]-2,3,3a,4,5,6-hexahydro-1H-
benz[de]isoquinolin-1-one chloride
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.4972(7)
_cell_length_b                   9.0288(8)
_cell_length_c                   25.045(2)
_cell_measurement_reflns_used    8390
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      27.73
_cell_measurement_theta_min      2.39
_cell_volume                     1695.3(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
;
SHELXTL/PC (Sheldrick, 1990), DIAMOND (Brandenburg & Putz, 2005)
and MERCURY (Macrae <i>et al.</i>,  2006)
;
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       \w
_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  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0178
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            12219
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.232
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.185
_refine_diff_density_min         -0.123
_refine_ls_abs_structure_details
'Flack & Bernardinelli (2000), with how many Friedel pairs?'
_refine_ls_abs_structure_Flack   -0.14(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         2980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0277
_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^)+(0.0386P)^2^+0.2731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0731
_reflns_number_gt                2914
_reflns_number_total             2980
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gk2050.cif
_cod_data_source_block           I
_cod_database_code               2212555
_cod_database_fobs_code          2212555