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_4503093
_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            'C6 H8 B2 I2 N4'
_chemical_formula_weight         411.58
_chemical_name_systematic        2,6-diiodopyrazabole
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 117.810(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.493(3)
_cell_length_b                   4.4270(10)
_cell_length_c                   13.654(2)
_cell_measurement_temperature    295
_cell_volume                     1256.0(4)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0785
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            1913
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.01
_diffrn_source                   'sealed tube'
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.976
_exptl_absorpt_correction_T_max  0.432
_exptl_absorpt_correction_T_min  0.334
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 Siemens SADABS 
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Prism '
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.361
_refine_diff_density_min         -0.991
_refine_diff_density_rms         0.191
_refine_ls_extinction_coef       0.0248(15)
_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   1.160
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         1423
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+9.2890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1432
_reflns_number_gt                1073
_reflns_number_total             1423
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg0702939-file003.cif
_cod_data_source_block           compound_3
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4503093