Crystal structure of 1-methoxy-2,2,2-tris(pyrazol-1-yl)ethane
Lyubartseva, Ganna; Parkin, Sean; Coleman, Morgan D.; Mallik, Uma Prasad; Acta Crystallographica Section E 70 (2014) o1047–o1048; doi:10.1107/S1600536814018789

data_2239931
_publ_section_title
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 Crystal structure of 1-methoxy-2,2,2-tris(pyrazol-1-yl)ethane
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_journal_coeditor_code           SU2774
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1047
_journal_page_last               o1048
_journal_paper_doi               10.1107/S1600536814018789
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C12 H14 N6 O'
_chemical_formula_moiety         'C12 H14 N6 O'
_chemical_formula_sum            'C12 H14 N6 O'
_chemical_formula_weight         258.29
_chemical_name_systematic
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1-Methoxy-2,2,2-tris(pyrazol-1-yl)ethane
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 102.5635(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5828(3)
_cell_length_b                   12.3847(3)
_cell_length_c                   8.4807(2)
_cell_measurement_reflns_used    1549
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1289.94(5)
_computing_cell_refinement       '<i>SCALEPACK</i> (Otwinowski & Minor, 1997)'
_computing_data_collection       '<i>COLLECT</i> (Nonius, 1998)'
_computing_data_reduction        '<i>DENZO-SMN</i> (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    '<i>XP in SHELXTL</i> (Sheldrick, 2008)'
_computing_publication_material
'<i>SHELXL2014</i> (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  '<i>SHELXL2014</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 9.1
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans at fixed \c = 55\%'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11397
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_min         2.335
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.232
_refine_diff_density_min         -0.178
_refine_ls_abs_structure_details
;
Refined as a perfect (<i>i.e.</i> 50:50) inversion twin.
;
_refine_ls_extinction_coef       0.0127(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     '<i>SHELXL2014</i> (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2934
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+0.5917P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.1024
_reflns_number_gt                2386
_reflns_number_total             2934
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su2774sup1.cif
_cod_data_source_block           I
_cod_database_code               2239931
_cod_database_fobs_code          2239931
_shelx_estimated_absorpt_t_min   0.975
_shelx_estimated_absorpt_t_max   0.985
_shelx_hkl_checksum              15813
_shelx_res_checksum              4752
_shelxl_version_number           2.014