A Complexation Study of 2,6-Bis(1-(p-tolyl)-1H-1,2,3-triazol-4-yl)pyridine Using Single-Crystal X-ray Diffraction and TRLFS.
Kiefer, Claude; Wagner, Anna T.; Beele, Björn B; Geist, Andreas; Panak, Petra J.; Roesky, Peter W.; Inorganic chemistry 54 (2015) 7301–7308; doi:10.1021/acs.inorgchem.5b00803

data_4343958
_publ_contact_author
;
      Prof. Dr. Peter W. Roesky
      Karlsruher Institut fuer Technologie (KIT), CS
      Institut fuer Anorganische Chemie (AOC)
      Lehrstuhl fuer Anorganische Funktionsmaterialien
      Engesserstr. 15, Geb. 30.45
      76131 Karlsruhe 
      Bundesrepublik Deutschland
;
_publ_section_title
;
 A Complexation Study of
 2,6-Bis(1-(p-tolyl)-1H-1,2,3-triazol-4-yl)pyridine Using Single-Crystal
 X-ray Diffraction and TRLFS.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7301
_journal_page_last               7308
_journal_paper_doi               10.1021/acs.inorgchem.5b00803
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C69 H57 Eu N21, 3(C F3 O3 S)'
_chemical_formula_sum            'C72 H57 Eu F9 N21 O9 S3'
_chemical_formula_weight         1779.52
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-10-07
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                71.259(6)
_cell_angle_beta                 88.315(6)
_cell_angle_gamma                88.557(6)
_cell_formula_units_Z            2
_cell_length_a                   13.6887(10)
_cell_length_b                   16.4306(12)
_cell_length_c                   18.8102(15)
_cell_measurement_reflns_used    11860
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.97
_cell_measurement_theta_min      1.86
_cell_volume                     4004.1(5)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2005)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED & LANA, PLATON (A.L.Spek, 2005)'
_computing_molecular_graphics    'Diamond 2/3, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'MS Word, Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Dectris Pilatus 100k'
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       '4-circle goniometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5mm monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1394
_diffrn_reflns_av_unetI/netI     0.1702
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37880
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.150
_diffrn_reflns_theta_min         1.897
_diffrn_source                   'Mo LFF Sealed Tube'
_diffrn_source_type              'Xenocs Genix3D microfocus'
_exptl_absorpt_coefficient_mu    0.950
_exptl_absorpt_correction_T_max  0.8776
_exptl_absorpt_correction_T_min  0.7448
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-Red, X-Shape & LANA'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       plate
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.227
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.076
_refine_diff_density_max         4.571
_refine_diff_density_min         -1.419
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1078
_refine_ls_number_reflns         15768
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.1241
_refine_ls_R_factor_gt           0.0805
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0907P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1834
_refine_ls_wR_factor_ref         0.2009
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9338
_reflns_number_total             15768
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00803_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 4343958.cif.'
_cod_database_code               4343958
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S2A-C71 = S2B-C71 = S3A-C72A = S3B-C72B
 1.775 with sigma of 0.002
3. Rigid bond restraints
 C70, S1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(S2A) = Uanis(S2B)
Uanis(O5A) = Uanis(O5B)
Uanis(F4A) = Uanis(F4B)
Uanis(F5A) = Uanis(F5B)
Uanis(F6A) = Uanis(F6B)
Uanis(O8A) = Uanis(O8B)
Uanis(O9A) = Uanis(O9B)
Uanis(S3A) = Uanis(S3B)
Uanis(F9A) = Uanis(F9B)
Uanis(F8A) = Uanis(F8B)
Uanis(F7A) = Uanis(F7B)
Uanis(C72A) = Uanis(C72B)
5. Others
 Fixed Sof: S2A(0.85) S2B(0.15) F4B(0.15) F5B(0.15) F6A(0.85) O5A(0.85)
 O5B(0.15) S3A(0.75) S3B(0.25) F7A(0.75) F8B(0.75) F9B(0.75) O8A(0.75)
 O8B(0.25) O9B(0.25) C72B(0.25) F7B(0.25) F6B(0.15) F5A(0.85) F4A(0.85)
 F8A(0.25) F9A(0.25) O9A(0.75) C72A(0.75)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C6(H6), C9(H9), C11(H11), C12(H12), C14(H14),
 C15(H15), C18(H18), C19(H19), C21(H21), C22(H22), C24(H24), C27(H27), C28(H28),
  C29(H29), C32(H32), C34(H34), C35(H35), C37(H37), C38(H38), C41(H41),
 C42(H42), C44(H44), C45(H45), C47(H47), C50(H50), C51(H51), C52(H52), C55(H55),
  C57(H57), C58(H58), C60(H60), C61(H61), C64(H64), C65(H65), C67(H67), C68(H68)
6.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C23(H23A,H23B,H23C), C39(H39A,H39B,H39C), C46(H46A,H46B,
 H46C), C62(H62A,H62B,H62C), C69(H69A,H69B,H69C)
;
_shelx_res_checksum              66866
_shelx_hkl_checksum              66837
_shelx_fab_checksum              17884
_olex2_submission_special_instructions 'No special instructions were received'