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_4127009
_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 Dy2 F36 N6 O12, C7 H8'
_chemical_formula_sum            'C49 H22 Dy2 F36 N6 O12'
_chemical_formula_weight         1895.72
_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                85.173(2)
_cell_angle_beta                 74.554(2)
_cell_angle_gamma                84.954(2)
_cell_formula_units_Z            1
_cell_length_a                   9.4160(4)
_cell_length_b                   11.0617(5)
_cell_length_c                   15.4355(7)
_cell_measurement_reflns_used    9080
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      70.074
_cell_measurement_theta_min      2.976
_cell_volume                     1540.55(12)
_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    'SHELXTL (Sheldrick, 2008-2013)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008-2013)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008-2013)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008-2013)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_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            46373
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.365
_diffrn_reflns_theta_min         2.976
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.439
_exptl_absorpt_correction_T_max  0.6479
_exptl_absorpt_correction_T_min  0.2622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1028 before and 0.0653 after correction. The Ratio of minimum to maximum transmission is 0.4047. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'orangish yellow'
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.043
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             910
_exptl_crystal_size_max          0.159
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         5842
_refine_ls_number_restraints     352
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+0.5418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0494
_refine_ls_wR_factor_ref         0.0499
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5671
_reflns_number_total             5842
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b12495_si_002.cif
_cod_data_source_block           compound_1-Dy
_cod_database_code               4127009
_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
 C15-C14 \\sim C15A-C14
 with sigma of 0.01
 F13-C11 \\sim F14-C11 \\sim F13A-C11A \\sim F14A-C11A \\sim F15-C11 \\sim
F15A-C11A
 with sigma of 0.01
 F16A-C15A \\sim F16-C15 \\sim F17A-C15A \\sim F17-C15 \\sim F18-C15 \\sim
F18A-C15A \\sim F10A-C10 ~
 F10-C10 \\sim F12-C10 \\sim F12A-C10 \\sim F11-C10 \\sim F11A-C10 \\sim
F14-C11 \\sim F13A-C11A \\sim F13-
 C11 \\sim F15A-C11A \\sim F15-C11 \\sim F14A-C11A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F16 \\sim F17 \\sim F18 \\sim C15 \\sim F16A \\sim F17A \\sim F18A \\sim C15A:
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01
F13 \\sim F14 \\sim F15 \\sim C11 \\sim F13A \\sim F14A \\sim F15A \\sim C11A:
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C11) = Uanis(C11A)
4. Others
 Sof(F16A)=Sof(F17A)=Sof(F18A)=Sof(C15A)=1-FVAR(1)
 Sof(F16)=Sof(F17)=Sof(F18)=Sof(C15)=FVAR(1)
 Sof(F13A)=Sof(F14A)=Sof(F15A)=Sof(C11A)=1-FVAR(2)
 Sof(F13)=Sof(F14)=Sof(F15)=Sof(C11)=FVAR(2)
 Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(3)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(3)
 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:
 C3(H3), C8(H8), C13(H13), C16(H16), C17(H17), C18(H18), C19(H19), C1S(H1S),
 C2S(H2S), C3S(H3S)
5.b Idealised Me refined as rotating group:
 C4S(H4SA,H4SB,H4SC)
;
_shelx_res_checksum              53112
_shelx_hkl_checksum              62098
_olex2_date_sample_data_collection 2016-12-23
_olex2_date_sample_submission    2016-12-23
_olex2_submission_special_instructions 'No special instructions were received'