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_4503096
_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                 100.205(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.974(3)
_cell_length_b                   9.604(4)
_cell_length_c                   5.5258(10)
_cell_measurement_reflns_used    4077
_cell_measurement_temperature    295
_cell_measurement_theta_max      28.5624
_cell_measurement_theta_min      3.7111
_cell_volume                     573.2(3)
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      295
_diffrn_detector_area_resol_mean 16.3990
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
  1 omega  -53.00    1.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.1177   75.0000  240.0000    0.0000    0.0000 54

  2 omega  -47.00    4.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.1177   48.0000  -13.0000    0.0000    0.0000 51

  3 omega  -43.00   11.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.1177  -75.0000    0.0000    0.0000    0.0000 54

  4 omega  -51.00    1.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865  -45.0000  240.0000    0.0000    0.0000 52

  5 omega  -51.00    4.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865  -75.0000  120.0000    0.0000    0.0000 55

  6 omega  -11.00   44.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865   75.0000    0.0000    0.0000    0.0000 55

  7 phi   -150.00  -88.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   21.5865    0.0000     -        0.0000    0.0000 62

  8 omega   -6.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865   45.0000  120.0000    0.0000    0.0000 52

  9 omega   42.00   94.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865   45.0000  240.0000    0.0000    0.0000 52

 10 omega    0.00   54.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865  -75.0000  120.0000    0.0000    0.0000 54

 11 omega   40.00   94.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865   75.0000    0.0000    0.0000    0.0000 54

 12 omega   -6.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865   45.0000  240.0000    0.0000    0.0000 52

 13 omega   -6.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865   45.0000    0.0000    0.0000    0.0000 52

 14 phi     -2.00   62.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -21.1177    0.0000     -        0.0000    0.0000 64

 15 phi    -32.00   32.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -21.1177    0.0000     -        0.0000    0.0000 64

 16 phi     28.00   92.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -21.1177    0.0000     -        0.0000    0.0000 64

 17 phi    -32.00   32.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   21.5865    0.0000     -        0.0000    0.0000 64

 18 phi    -62.00    2.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   21.5865    0.0000     -        0.0000    0.0000 64

 19 phi     58.00  122.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   21.5865    0.0000     -        0.0000    0.0000 64

 20 phi   -122.00  -58.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   21.5865    0.0000     -        0.0000    0.0000 64

;
_diffrn_orient_matrix_UB_11      0.0020683485
_diffrn_orient_matrix_UB_12      -0.0249378516
_diffrn_orient_matrix_UB_13      -0.1199368308
_diffrn_orient_matrix_UB_21      -0.0154539691
_diffrn_orient_matrix_UB_22      -0.0676640396
_diffrn_orient_matrix_UB_23      0.0358052426
_diffrn_orient_matrix_UB_31      -0.0637341704
_diffrn_orient_matrix_UB_32      0.0155513059
_diffrn_orient_matrix_UB_33      -0.0362978478
_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  0.0178
_diffrn_reflns_av_sigmaI/netI    0.0082
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            5818
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.952
_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    1.621
_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          0.25
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.220
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.032
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         691
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0448P)^2^+0.1723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0825
_reflns_number_gt                588
_reflns_number_total             691
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg0702939-file003.cif
_cod_data_source_block           compound_6
_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_sg_symbol_H-M      C2/m
_cod_database_code               4503096