Supramolecular organization of perfluorinated 1H-indazoles in the solid state using X-ray crystallography, SSNMR and sensitive (VCD) and non sensitive (MIR, FIR and Raman) to chirality vibrational spectroscopies.
Quesada-Moreno, María M; Avilés-Moreno, Juan Ramón; López-González, Juan Jesús; Jacob, Kane; Vendier, Laure; Etienne, Michel; Alkorta, Ibon; Elguero, José; Claramunt, Rosa M.; Physical chemistry chemical physics : PCCP 19 (2017) 1632–1643; doi:10.1039/c6cp04940k

data_7227210
_publ_section_title
;
 Supramolecular organization of perfluorinated 1H-indazoles in the solid
 state using X-ray crystallography, SSNMR and sensitive (VCD) and non
 sensitive (MIR, FIR and Raman) to chirality vibrational spectroscopies.
;
_journal_issue                   2
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              1632
_journal_page_last               1643
_journal_paper_doi               10.1039/c6cp04940k
_journal_volume                  19
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C9 H1 F9 N2'
_chemical_formula_sum            'C9 H F9 N2'
_chemical_formula_weight         308.10
_space_group_IT_number           145
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 32'
_symmetry_space_group_name_H-M   'P 32'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2016-10-24 deposited with the CCDC.
2016-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   12.3863(7)
_cell_length_b                   12.3863(7)
_cell_length_c                   5.5727(3)
_cell_measurement_reflns_used    9865
_cell_measurement_temperature    100
_cell_measurement_theta_max      72
_cell_measurement_theta_min      4
_cell_volume                     740.42(7)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.056
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            16067
_diffrn_reflns_theta_full        72.292
_diffrn_reflns_theta_max         72.292
_diffrn_reflns_theta_min         4.121
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.284
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.41
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.073
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             450
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.24
_refine_diff_density_min         -0.26
_refine_ls_abs_structure_details 'Flack (1983), 952 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.22(10)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9188
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         1919
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.0074740
_refine_ls_shift/su_mean         0.0006432
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 0.42P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0688
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0688
_reflns_limit_h_max              7
_reflns_limit_h_min              -15
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              6
_reflns_limit_l_min              -6
_reflns_number_gt                1904
_reflns_number_total             1926
_reflns_threshold_expression     I>2.0\s(I)
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT ENANTIO 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
_cod_data_source_file            c6cp04940k2.cif
_cod_data_source_block           CF2CF3microCu
_cod_depositor_comments
'Adding full bibliography for 7227208--7227210.cif.'
_cod_original_sg_symbol_H-M      'P 32 '
_cod_original_formula_sum        'C9 H1 F9 N2'
_cod_database_code               7227210