4,5,6,7,8,9-Hexahydro-2<i>H</i>-cycloocta[<i>c</i>]pyrazol-1-ium-3-olate
Fun, Hoong-Kun; Yeap, Chin Sing; Ragavan, R. Venkat; Vijayakumar, V.; Sarveswari, S.; Acta Crystallographica Section E 66 (2010) o3019–; doi:10.1107/S1600536810043904

data_2227434
_publ_section_title
;
 4,5,6,7,8,9-Hexahydro-2<i>H</i>-cycloocta[<i>c</i>]pyrazol-1-ium-3-olate
;
_journal_coeditor_code           FJ2356
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3019
_journal_paper_doi               10.1107/S1600536810043904
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C9 H14 N2 O'
_chemical_formula_moiety         'C9 H14 N2 O'
_chemical_formula_sum            'C9 H14 N2 O'
_chemical_formula_weight         166.22
_chemical_name_systematic
;
4,5,6,7,8,9-Hexahydro-2<i>H</i>-cycloocta[<i>c</i>]pyrazol-1-ium-3-olate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 111.6200(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8078(2)
_cell_length_b                   6.77580(10)
_cell_length_c                   10.7096(2)
_cell_measurement_reflns_used    3802
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.06
_cell_measurement_theta_min      3.46
_cell_volume                     864.03(3)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6990
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.9909
_exptl_absorpt_correction_T_min  0.9556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.254
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         1680
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0470P)^2^+0.3516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                1474
_reflns_number_total             1680
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fj2356.cif
_cod_data_source_block           I
_cod_original_cell_volume        864.03(2)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2227434
_cod_database_fobs_code          2227434