3(5),4-Dimethyl- and 3,4,5-trimethylpyrazole at 200K. X-ray crystallography and quantum-chemical analysis
Infantes, L.; Foces-Foces, C.; Elguero,J.; Acta Crystallographica Section B 55 (1999) 441–447; doi:10.1107/S0108768198014013

data_2002947
_publ_section_title
;
 3(5),4-Dimethyl- and 3,4,5-trimethylpyrazole at 200K. X-ray
 crystallography and quantum-chemical analysis
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              441
_journal_page_last               447
_journal_paper_doi               10.1107/S0108768198014013
_journal_volume                  55
_journal_year                    1999
_chemical_formula_moiety         'C6 H10 N2'
_chemical_formula_sum            'C6 H10 N2'
_chemical_formula_weight         110.2
_chemical_melting_point          .411E-305
_chemical_name_systematic        3,4,5-trimethylpyrazole
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_cell_angle_alpha                90.00000
_cell_angle_beta                 90.696(9)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            12
_cell_length_a                   14.1911(9)
_cell_length_b                   8.2520(6)
_cell_length_c                   16.7382(19)
_cell_measurement_reflns_used    43
_cell_measurement_temperature    200
_cell_measurement_theta_max      45.0
_cell_measurement_theta_min      5.2
_cell_volume                     1960.0(3)
_computing_cell_refinement       'LSUCRE (Appleman, 1984)'
_computing_data_collection       'Philips PW1100 (Hornstra & Vossers, 1973)'
_computing_data_reduction        xtal_DIFDAT_SORTRF_ADDREF
_computing_molecular_graphics    xtal_ORTEP
_computing_publication_material  xtal_BONDLA_CIFIO
_computing_structure_refinement  'xtal_CRYLSQ (Hall et al., 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_measurement_device       'Philips PW1100 diffractometer'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         xray_tube
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  .024
_diffrn_reflns_av_sigmaI/netI    .013
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1863
_diffrn_reflns_reduction_process perpendicular_monochr_Lp
_diffrn_reflns_theta_max         65.08
_diffrn_reflns_theta_min         5.29
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  90
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.546
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.12
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Rectangular prism'
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.67
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.22
_refine_diff_density_min         -0.20
_refine_ls_abs_structure_details none
_refine_ls_extinction_coef       390.(10)
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_all   .913
_refine_ls_goodness_of_fit_obs   .887
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     182
_refine_ls_number_reflns         1366
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .059
_refine_ls_R_factor_obs          .048
_refine_ls_shift/esd_max         .07
_refine_ls_shift/esd_mean        .006
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = k/[(A+B Fo)^2^(C+D(sin\q)/\l)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .063
_refine_ls_wR_factor_obs         .054
_reflns_number_observed          1372
_reflns_number_total             1680
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            bm0017.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '411-412' was changed to '411.5(5)' -
the average value was taken and precision was
estimated.

'_geom_hbond_publ_flag' value 'Yes' changed to 'yes'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (3
times).

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

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = k/[(A+B
Fo)^2^(C+D(sin\q)/\l)]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = k/[(A+B Fo)^2^(C+D(sin\q)/\l)]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               2002947
_cod_database_fobs_code          2002947