Perfluorinated 1H-indazoles and hydrotris(indazol-1-yl)borates. Supramolecular organization and a new synthetic procedure to form scorpionate ligands
Muñoz, Bianca K.; Ojo, Wilfried-Solo; Jacob, Kane; Romero, Nuria; Vendier, Laure; Despagnet-Ayoub, Emmanuelle; Etienne, Michel; New Journal of Chemistry 38 (2014) 2451–; doi:10.1039/c4nj00136b

data_7054255
_publ_section_title
;
 Perfluorinated 1H-indazoles and hydrotris(indazol-1-yl)borates.
 Supramolecular organization and a new synthetic procedure to form
 scorpionate ligands
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2451
_journal_paper_doi               10.1039/c4nj00136b
_journal_volume                  38
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C13 H F17 N2'
_chemical_formula_sum            'C13 H F17 N2'
_chemical_formula_weight         508.16
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 99.598(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1749(9)
_cell_length_b                   6.3085(5)
_cell_length_c                   18.2579(16)
_cell_measurement_reflns_used    3505
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      29.1224
_cell_measurement_theta_min      3.3727
_cell_measurement_wavelength     0.71073
_cell_volume                     1609.8(2)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
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        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 16.1978
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0255596
_diffrn_orient_matrix_UB_12      0.0692317
_diffrn_orient_matrix_UB_13      -0.0267968
_diffrn_orient_matrix_UB_21      0.001324
_diffrn_orient_matrix_UB_22      0.0800217
_diffrn_orient_matrix_UB_23      0.0275154
_diffrn_orient_matrix_UB_31      0.0438102
_diffrn_orient_matrix_UB_32      0.0379743
_diffrn_orient_matrix_UB_33      -0.008852
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0739
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13951
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.38
_exptl_absorpt_coefficient_mu    0.265
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.097
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.863
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         3287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.863
_refine_ls_R_factor_all          0.1125
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0796P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1395
_reflns_number_gt                1638
_reflns_number_total             3287
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4nj00136b1.cif
_cod_data_source_block           5
_cod_original_formula_sum        'C13 H F17 N2 '
_cod_database_code               7054255