Crystal structure of 3-methyl-5-trimethylsilyl-1<i>H</i>-pyrazole
Ferrence, Gregory M.; Kocher, Joshua L.; Acta Crystallographica Section E 71 (2015) o397–; doi:10.1107/S2056989015008567

data_2240632
_publ_section_title
;
 Crystal structure of 3-methyl-5-trimethylsilyl-1<i>H</i>-pyrazole
;
_journal_coeditor_code           ZL2621
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o397
_journal_paper_doi               10.1107/S2056989015008567
_journal_volume                  71
_journal_year                    2015
_chemical_formula_moiety         'C7 H14 N2 Si'
_chemical_formula_sum            'C7 H14 N2 Si'
_chemical_formula_weight         154.29
_chemical_name_systematic
;
3-Methyl-5-trimethylsilyl-1<i>H</i>-pyrazole
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   iterative
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   19.221(3)
_cell_length_b                   19.221
_cell_length_c                   10.5812(18)
_cell_measurement_reflns_used    6620
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.97
_cell_measurement_theta_min      2.2
_cell_volume                     3909.2(9)
_computing_cell_refinement
;
APEX2 and SAINT (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and
<i>Mercury</i> (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
<i>WinGX</i> (Farrugia, 2012) and <i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SUPERFLIP (Palatinus & Chapuis, 2007)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
;
Bruker SMART APEX CCD
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14542
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.474
_diffrn_reflns_theta_min         2.119
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.179
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.4996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(APEX; Bruker, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.049
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.278
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     100
_refine_ls_number_reflns         2240
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+6.7007P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1211
_reflns_number_gt                1811
_reflns_number_total             2240
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zl2621sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        3909.4(15)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               2240632