The Boat Conformation in Pyrazaboles. A Theoretical and Experimental Study†
Cavero, Emma; Giménez, Raquel; Uriel, Santiago; Beltrán, Eduardo; Serrano, José Luis; Alkorta, Ibon; Elguero, José; Crystal Growth & Design 8 (2008) 838–; doi:10.1021/cg0702939

data_4503097
_publ_section_title
;
 The Boat Conformation in Pyrazaboles. A Theoretical and Experimental
 Study&#x2020;
;
_journal_issue                   3
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              838
_journal_paper_doi               10.1021/cg0702939
_journal_volume                  8
_journal_year                    2008
_chemical_formula_sum            'C10 H6 B2 F4 N4'
_chemical_formula_weight         279.81
_chemical_name_systematic        4,4,8,8-tetrafluoro-2,6-bis(ethynyl)pyrazabole
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 101.39(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.9005(18)
_cell_length_b                   9.5590(19)
_cell_length_c                   5.461(3)
_cell_measurement_reflns_used    2338
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.5813
_cell_measurement_theta_min      3.7928
_cell_volume                     557.8(3)
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 16.3990
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -48.00    4.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.1177   45.0000    0.0000    0.0000    0.0000 52

  2 omega  -73.00  -27.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.1177  111.0000  -50.0000    0.0000    0.0000 46

  3 omega  -51.00    1.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865  -45.0000    0.0000    0.0000    0.0000 52

  4 omega    1.00   45.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865 -130.0000  293.0000    0.0000    0.0000 44

  5 omega   -6.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865   45.0000    0.0000    0.0000    0.0000 52

  6 omega   -3.00   49.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865  -45.0000    0.0000    0.0000    0.0000 52

  7 omega    0.00   54.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865  -75.0000  120.0000    0.0000    0.0000 54

  8 phi     -2.00   62.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   21.5865    0.0000     -        0.0000    0.0000 64

  9 phi    -62.00    2.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -21.1177    0.0000     -        0.0000    0.0000 64

 10 phi    -92.00  -28.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   21.5865    0.0000     -        0.0000    0.0000 64

 11 phi   -180.00 -118.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   21.5865    0.0000     -        0.0000    0.0000 62

 12 phi     88.00  113.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   21.5865    0.0000     -        0.0000    0.0000 25

;
_diffrn_orient_matrix_UB_11      -0.0091797710
_diffrn_orient_matrix_UB_12      0.0087755392
_diffrn_orient_matrix_UB_13      0.1238366218
_diffrn_orient_matrix_UB_21      0.0126455817
_diffrn_orient_matrix_UB_22      -0.0717356209
_diffrn_orient_matrix_UB_23      0.0240713617
_diffrn_orient_matrix_UB_31      0.0644556438
_diffrn_orient_matrix_UB_32      0.0154503607
_diffrn_orient_matrix_UB_33      0.0398497271
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0183
_diffrn_reflns_av_sigmaI/netI    0.0112
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            2970
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    0.149
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.961
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
?
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+0.2785P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0731
_reflns_number_gt                532
_reflns_number_total             605
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg0702939-file003.cif
_cod_data_source_block           compound_6150K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_cell_volume        557.8(4)
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               4503097