Lanthanide Triangles Supported by Radical Bridging Ligands.
Dolinar, Brian S.; Alexandropoulos, Dimitris I.; Vignesh, Kuduva R.; James, Tia'Asia; Dunbar, Kim R.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b12495

data_4127008
_publ_section_title
;
 Lanthanide Triangles Supported by Radical Bridging Ligands.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b12495
_journal_year                    2017
_chemical_formula_moiety         'C42 H14 F36 N6 O12 Y2, C7 H8'
_chemical_formula_sum            'C49 H22 F36 N6 O12 Y2'
_chemical_formula_weight         1748.54
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                85.234(17)
_cell_angle_beta                 74.48(2)
_cell_angle_gamma                84.902(16)
_cell_formula_units_Z            1
_cell_length_a                   9.405(7)
_cell_length_b                   11.044(9)
_cell_length_c                   15.445(11)
_cell_measurement_reflns_used    9857
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      25.726
_cell_measurement_theta_min      2.374
_cell_volume                     1537(2)
_computing_cell_refinement       'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_data_collection       'APEX3(Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTON area detector'
_diffrn_measurement_method       '0.5\ \w and 0.5\ \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33789
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.772
_diffrn_reflns_theta_max         25.772
_diffrn_reflns_theta_min         2.253
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.052
_exptl_absorpt_correction_T_max  0.9398
_exptl_absorpt_correction_T_min  0.5661
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1377 before and 0.0564 after correction. The Ratio of minimum to maximum transmission is 0.6024. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.889
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.276
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         5884
_refine_ls_number_restraints     375
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+1.1325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0741
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5227
_reflns_number_total             5884
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b12495_si_002.cif
_cod_data_source_block           Compound_1-Y
_cod_database_code               4127008
_shelx_shelxl_version_number     2016/6
_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
 C34A-C12 \\sim C11-C12 \\sim C14-C43A \\sim C14-C15
 with sigma of 0.01
 F13A-C34A \\sim F15A-C34A \\sim F15-C11 \\sim F13-C11 \\sim F14A-C34A \\sim
F14-C11 \\sim F17-C15 ~
 F17A-C43A \\sim F18-C15 \\sim F18A-C43A \\sim F16-C15 \\sim F16A-C43A \\sim
F11-C10 \\sim F11A-C10 ~
 F12A-C10 \\sim F12-C10 \\sim F10-C10 \\sim F10A-C10
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F18 \\sim F17 \\sim C15 \\sim F16 \\sim F17A \\sim F18A \\sim F16A \\sim C43A:
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01
F14 \\sim F15 \\sim C11 \\sim F13 \\sim F14A \\sim C34A \\sim F15A \\sim F13A:
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01
F12A \\sim F12 \\sim F11A \\sim F11 \\sim F10A \\sim F10: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Sof(F14A)=Sof(C34A)=Sof(F15A)=Sof(F13A)=1-FVAR(1)
 Sof(F14)=Sof(F15)=Sof(C11)=Sof(F13)=FVAR(1)
 Sof(F11)=Sof(F10)=Sof(F12)=1-FVAR(2)
 Sof(F11A)=Sof(F12A)=Sof(F10A)=FVAR(2)
 Sof(F17A)=Sof(F18A)=Sof(F16A)=1-FVAR(3)
 Sof(F18)=Sof(F17)=Sof(F16)=FVAR(3)
 Sof(C43A)=1-FVAR(4)
 Sof(C15)=FVAR(4)
 Fixed Sof: H3S(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5) H4SC(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C3(H3), C17(H17), C19(H19), C16(H16), C8(H8), C13(H13), C1S(H1S),
 C2S(H2S), C3S(H3S)
5.b Idealised Me refined as rotating group:
 C4S(H4SA,H4SB,H4SC)
;
_shelx_res_checksum              36543
_shelx_hkl_checksum              78190
_olex2_submission_special_instructions 'No special instructions were received'