3,5,3',5'-Tetramethyl-4,4'-bi(1<i>H</i>-pyrazolyl) hemihydrate
Jin, Shouwen; Huang, Yanfei; Fang, Hao; Wang, Tianyi; Ding, Liangliang; Acta Crystallographica Section E 68 (2012) o2896–; doi:10.1107/S1600536812037920

data_2236514
_publ_section_title
;
 3,5,3',5'-Tetramethyl-4,4'-bi(1<i>H</i>-pyrazolyl) hemihydrate
;
_journal_coeditor_code           NG5290
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2896
_journal_paper_doi               10.1107/S1600536812037920
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C10 H14 N4, 0.5H2 O'
_chemical_formula_moiety         'C10 H14 N4, 0.5(H2 O)'
_chemical_formula_sum            'C10 H15 N4 O0.5'
_chemical_formula_weight         199.26
_chemical_name_systematic
;
3,5,3',5'-Tetramethyl-4,4'-bi(1<i>H</i>-pyrazolyl) hemihydrate
;
_space_group_IT_number           142
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2c'
_symmetry_space_group_name_H-M   'I 41/a c d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            32
_cell_length_a                   24.9060(4)
_cell_length_b                   24.9060
_cell_length_c                   14.9684(2)
_cell_measurement_reflns_used    3432
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.3656
_cell_measurement_theta_min      2.5809
_cell_volume                     9285.03(19)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_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 1K CCD area-detector'
_diffrn_measurement_method       '\f and \w 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  0.0698
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27495
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  0.9726
_exptl_absorpt_correction_T_min  0.9704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3424
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2050
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0974P)^2^+1.8190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1510
_refine_ls_wR_factor_ref         0.1690
_reflns_number_gt                1480
_reflns_number_total             2050
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ng5290.cif
_cod_data_source_block           I
_cod_original_cell_volume        9285.0(2)
_cod_original_sg_symbol_Hall     '-I  4bd 2c'
_cod_original_sg_symbol_H-M      'I 41/acd'
_cod_database_code               2236514
_cod_database_fobs_code          2236514