Crystal structure of 1,4,5,6,7,8,9,10,11,12,13-undecahydrocyclododeca[<i>c</i>]pyrazol-3-ol
Raymond, Casey C.; Knopp, Michael A.; Acta Crystallographica Section E 71 (2015) o752–o753; doi:10.1107/S2056989015016746

data_2241085
_publ_section_title
;
 Crystal structure of
 1,4,5,6,7,8,9,10,11,12,13-undecahydrocyclododeca[<i>c</i>]pyrazol-3-ol
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o752
_journal_page_last               o753
_journal_paper_doi               10.1107/S2056989015016746
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C13 H22 N2 O'
_chemical_formula_moiety         'C13 H22 N2 O'
_chemical_formula_sum            'C13 H22 N2 O'
_chemical_formula_weight         222.32
_chemical_name_systematic
;
1,4,5,6,7,8,9,10,11,12,13-Undecahydrocyclododeca[<i>c</i>]pyrazol-3-ol
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 105.4374(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.008(2)
_cell_length_b                   7.4764(5)
_cell_length_c                   11.6516(8)
_cell_measurement_reflns_used    9304
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.4989
_cell_measurement_theta_min      2.814
_cell_volume                     2519.7(3)
_computing_cell_refinement
;
SAINT (Bruker, 2007)
;
_computing_data_collection
;
APEX2 (Bruker, 2007)
;
_computing_data_reduction
;
SAINT (Bruker, 2007)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX CCD '
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14420
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.502
_diffrn_reflns_theta_min         2.814
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2007)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       plate
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.590
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         3845
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+2.2017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1193
_reflns_number_gt                3383
_reflns_number_total             3845
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su5204sup1.cif
_cod_data_source_block           I
_cod_database_code               2241085
_cod_database_fobs_code          2241085
_shelx_estimated_absorpt_t_min   0.957
_shelx_estimated_absorpt_t_max   0.992
_shelx_hkl_checksum              22344
_shelx_res_checksum              65154
_shelxl_version_number           2014/6