Synthesis of trifluoromethyl-substituted N-aryl-poly-1,2,3-triazole derivatives
Kumar, A. Sudheer; Kommu, Nagarjuna; Ghule, Vikas D.; Sahoo, Akhila K.; Journal of Materials Chemistry A 2 (2014) 7917–; doi:10.1039/c3ta15184k

data_7235383
_publ_section_title
;
 Synthesis of trifluoromethyl-substituted N-aryl-poly-1,2,3-triazole
 derivatives
;
_journal_issue                   21
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              7917
_journal_paper_doi               10.1039/c3ta15184k
_journal_volume                  2
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety
'0.13(C9 H6 Cl2 F3 N3), 0.13(C9 H4 Cl2 F3 N3)'
_chemical_formula_sum            'C H Cl F N'
_chemical_formula_weight         81.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-07-28
_audit_creation_method
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  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
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_cell_angle_alpha                90.00
_cell_angle_beta                 105.264(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   16.0332(12)
_cell_length_b                   6.8721(4)
_cell_length_c                   10.7030(7)
_cell_measurement_reflns_used    1414
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.3154
_cell_measurement_theta_min      2.8391
_cell_volume                     1137.67(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.3291
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   54.00   83.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7003  179.0000  150.0000 29

  2 omega  -51.00   38.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7003  -19.0000   60.0000 89

  3 omega  -54.00   49.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7003  -19.0000  150.0000 103
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0425126000
_diffrn_orient_matrix_UB_12      -0.0276734000
_diffrn_orient_matrix_UB_13      0.0006581000
_diffrn_orient_matrix_UB_21      0.0172099000
_diffrn_orient_matrix_UB_22      -0.0707437000
_diffrn_orient_matrix_UB_23      0.0481378000
_diffrn_orient_matrix_UB_31      0.0005643000
_diffrn_orient_matrix_UB_32      0.0698639000
_diffrn_orient_matrix_UB_33      0.0489787000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
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_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4462
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.96
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.071
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             640
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.18(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.586
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         2783
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.586
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0688
_refine_ls_shift/su_max          0.603
_refine_ls_shift/su_mean         0.113
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2048
_refine_ls_wR_factor_ref         0.2299
_reflns_number_gt                2153
_reflns_number_total             2783
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ta15184k2.cif
_cod_data_source_block           ak
_cod_original_cell_volume        1137.67(13)
_cod_database_code               7235383
_chemical_oxdiff_formula         'C H N F Cl'
_chemical_oxdiff_usercomment     sudheer
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32