Temperature dependence of the crystal structure of 3,5-di-<i>tert</i>-butylpyrazole from 10K
Sobolev, Alexandre N.; White, Allan H.; Acta Crystallographica Section B 60 (2004) 621–625; doi:10.1107/S0108768104017380

data_2102639
_publ_section_title
;
 Temperature dependence of the crystal structure of
 3,5-di-<i>tert</i>-butylpyrazole from 10K
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              621
_journal_page_last               625
_journal_paper_doi               10.1107/S0108768104017380
_journal_volume                  60
_journal_year                    2004
_chemical_formula_moiety         'C11 H20 N2'
_chemical_formula_sum            'C11 H20 N2'
_chemical_formula_weight         180.29
_chemical_name_common            3,5-di-tert-butylpyrazole
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P -2a -2ab'
_symmetry_space_group_name_H-M   'P b 21 a'
_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            16
_cell_length_a                   11.279(2)
_cell_length_b                   20.634(4)
_cell_length_c                   19.542(4)
_cell_measurement_reflns_used    14
_cell_measurement_temperature    10(2)
_cell_measurement_theta_max      20.1
_cell_measurement_theta_min      16.0
_cell_volume                     4548.0(15)
_computing_cell_refinement       'Local diffractometer control software'
_computing_data_collection       'Local diffractometer control software'
_computing_data_reduction        'PROFIT (Streltsov & Zavodnik, 1989)'
_computing_molecular_graphics    'SHELXTL (Bruker,1997)'
_computing_publication_material  'SHELXTL (Bruker,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      10(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Huber 512 goniometer'
_diffrn_measurement_method       '\w-2\q scan'
_diffrn_radiation_monochromator  none
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15825
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_T_max  0.9875
_exptl_absorpt_correction_T_min  0.9799
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
'XTAL 3.7 (Hall, du Boulay & Olthof-Hazekamp, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.053
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prism
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.213
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(3)
_refine_ls_extinction_coef       0.0012(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     742
_refine_ls_number_reflns         4162
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0639P)^2^+0.7985P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.1015
_reflns_number_gt                3744
_reflns_number_total             4162
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ta5008.cif
_cod_data_source_block           10k
_cod_depositor_comments
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The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
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_cod_database_code               2102639