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_4127012
_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
'2(C66 H30 Dy0.31 F36 N18 O12 Y2.69), 2(C4 H10 O)'
_chemical_formula_sum            'C140 H87 Dy0.65 F72 N36 O26 Y5.35'
_chemical_formula_weight         4638.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                90
_cell_angle_beta                 113.867(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.245(2)
_cell_length_b                   34.335(3)
_cell_length_c                   21.8451(18)
_cell_measurement_reflns_used    9675
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      23.67
_cell_measurement_theta_min      2.21
_cell_volume                     18002(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 Ver. 2014.1-1 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_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  0.0997
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            309942
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.768
_diffrn_reflns_theta_min         0.848
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.119
_exptl_absorpt_correction_T_max  0.7244
_exptl_absorpt_correction_T_min  0.6196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0721 before and 0.0617 after correction. The Ratio of minimum to maximum transmission is 0.8553. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9146
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.255
_exptl_crystal_size_min          0.242
_refine_diff_density_max         0.942
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2966
_refine_ls_number_reflns         34251
_refine_ls_number_restraints     3513
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0244P)^2^+39.1491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0955
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23816
_reflns_number_total             34251
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b12495_si_002.cif
_cod_data_source_block           Compound_2-DyY
_cod_database_code               4127012
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Dy2', Y2'}
{Y3', Dy3'}
{Y1', Dy1'}
{Y3, Dy3}
{Y1, Dy1}
{Y2, Dy2}
3. Restrained distances
 C7-C6 \\sim C7-C6A \\sim C15A-C14 \\sim C15-C14 \\sim C20'-C19' \\sim
C20"-C19' \\sim C24'-C25" ~
 C25'-C24' \\sim C5"-C4' \\sim C5'-C4'
 with sigma of 0.01
 F7A-C6A \\sim F7-C6 \\sim F8-C6 \\sim F8A-C6A \\sim F9-C6 \\sim F9A-C6A \\sim
F17A-C15A \\sim F17-C15 ~
 F18A-C15A \\sim F18-C15 \\sim F16-C15 \\sim F16A-C15A \\sim F13-C11 \\sim
F13A-C11 \\sim F15-C11 ~
 F15A-C11 \\sim F14-C11 \\sim F14A-C11 \\sim F22A-C20 \\sim F22-C20 \\sim
F24A-C20 \\sim F24-C20 \\sim F23-
 C20 \\sim F23A-C20 \\sim F30A-C25 \\sim F30-C25 \\sim F28A-C25 \\sim F28-C25
\\sim F29-C25 \\sim F29A-C25
 \\sim F32-C26 \\sim F32A-C26 \\sim F33A-C26 \\sim F33-C26 \\sim F31A-C26 \\sim
F31-C26 \\sim F18"-C15' ~
 F18'-C15' \\sim F16'-C15' \\sim F16"-C15' \\sim F17"-C15' \\sim F17'-C15'
\\sim F14"-C11' \\sim F14'-
 C11' \\sim F13"-C11' \\sim F13'-C11' \\sim F15"-C11' \\sim F15'-C11' \\sim
F24"-C20" \\sim F24'-C20' ~
 F22"-C20" \\sim F23"-C20" \\sim F23'-C20' \\sim F22'-C20' \\sim F29'-C25'
\\sim F29"-C25" \\sim F28"-
 C25" \\sim F28'-C25' \\sim F30"-C25" \\sim F30'-C25' \\sim F31"-C26' \\sim
F31'-C26' \\sim F33'-C26' ~
 F33"-C26' \\sim F32"-C26' \\sim F32'-C26' \\sim F5"-C5" \\sim F5'-C5' \\sim
F6"-C5" \\sim F6'-C5' ~
 F4'-C5' \\sim F4"-C5"
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
O2S \\sim C8S \\sim C7S \\sim C6S \\sim C5S \\sim O2SA \\sim C8SA \\sim C7SA
\\sim C6SA \\sim C5SA \\sim O1SA \\sim C4SA \\sim C3SA \\sim C2SA \\sim C1SA
\\sim O1S \\sim C4S \\sim C3S \\sim C2S \\sim C1S: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.01
F7 \\sim F8 \\sim F9 \\sim C6 \\sim F7A \\sim F8A \\sim F9A \\sim C6A: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01
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 F13A \\sim F14A \\sim F15A \\sim C11: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.01
F22 \\sim F23 \\sim F24 \\sim F22A \\sim F23A \\sim F24A: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.01
F28 \\sim F29 \\sim F30 \\sim F28A \\sim F29A \\sim F30A: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.01
F34 \\sim F31 \\sim F32 \\sim F33 \\sim F31A \\sim F32A \\sim F33A: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.01
F4' \\sim F5' \\sim F6' \\sim C5' \\sim F4" \\sim F5" \\sim F6" \\sim C5":
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01
F22' \\sim F23' \\sim F24' \\sim C20' \\sim F22" \\sim F23" \\sim F24" \\sim
C20": within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01
C11' \\sim F13' \\sim F14' \\sim F15' \\sim F13" \\sim F14" \\sim F15": within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01
F16' \\sim F17' \\sim F18' \\sim F16" \\sim F17" \\sim F18": within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.01
F28' \\sim F29' \\sim F30' \\sim C25' \\sim F28" \\sim F29" \\sim F30" \\sim
C25": within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01
F31' \\sim F32' \\sim F33' \\sim F31" \\sim F32" \\sim F33": within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(F13) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Dy2') = Uanis(Y2')
Uanis(Y3') = Uanis(Dy3')
Uanis(Y1') = Uanis(Dy1')
Uanis(Y3) = Uanis(Dy3)
Uanis(Y1) = Uanis(Dy1)
Uanis(Y2) = Uanis(Dy2)
5. Others
 Sof(Dy1)=Sof(Dy2)=Sof(Dy3)=Sof(Dy1')=Sof(Dy2')=Sof(Dy3')=1-FVAR(1)
 Sof(Y1)=Sof(Y2)=Sof(Y3)=Sof(Y1')=Sof(Y2')=Sof(Y3')=FVAR(1)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=Sof(C6A)=1-FVAR(2)
 Sof(F7)=Sof(F8)=Sof(F9)=Sof(C6)=FVAR(2)
 Sof(F13A)=Sof(F14A)=Sof(F15A)=1-FVAR(3)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(3)
 Sof(F16A)=Sof(F17A)=Sof(F18A)=Sof(C15A)=1-FVAR(4)
 Sof(F16)=Sof(F17)=Sof(F18)=Sof(C15)=FVAR(4)
 Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(5)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(5)
 Sof(F28A)=Sof(F29A)=Sof(F30A)=1-FVAR(6)
 Sof(F28)=Sof(F29)=Sof(F30)=FVAR(6)
 Sof(F31A)=Sof(F32A)=Sof(F33A)=1-FVAR(7)
 Sof(F31)=Sof(F32)=Sof(F33)=FVAR(7)
 Sof(F4")=Sof(F5")=Sof(F6")=Sof(C5")=1-FVAR(8)
 Sof(F4')=Sof(F5')=Sof(F6')=Sof(C5')=FVAR(8)
 Sof(F13")=Sof(F14")=Sof(F15")=1-FVAR(9)
 Sof(F13')=Sof(F14')=Sof(F15')=FVAR(9)
 Sof(F16")=Sof(F17")=Sof(F18")=1-FVAR(10)
 Sof(F16')=Sof(F17')=Sof(F18')=FVAR(10)
 Sof(F22")=Sof(F23")=Sof(F24")=Sof(C20")=1-FVAR(11)
 Sof(F22')=Sof(F23')=Sof(F24')=Sof(C20')=FVAR(11)
 Sof(F28")=Sof(F29")=Sof(F30")=Sof(C25")=1-FVAR(12)
 Sof(F28')=Sof(F29')=Sof(F30')=Sof(C25')=FVAR(12)
 Sof(F31")=Sof(F32")=Sof(F33")=1-FVAR(13)
 Sof(F31')=Sof(F32')=Sof(F33')=FVAR(13)
 Sof(O2SA)=Sof(C8SA)=Sof(H8SD)=Sof(H8SE)=Sof(H8SF)=Sof(C7SA)=Sof(H7SC)=
 Sof(H7SD)=Sof(C6SA)=Sof(H6SC)=Sof(H6SD)=Sof(C5SA)=Sof(H5SD)=Sof(H5SE)=
 Sof(H5SF)=Sof(O1SA)=Sof(C4SA)=Sof(H4SA)=Sof(H4SB)=Sof(H4SC)=Sof(C3SA)=
 Sof(H3SA)=Sof(H3SB)=Sof(C2SA)=Sof(H2SA)=Sof(H2SB)=Sof(C1SA)=Sof(H1SA)=
 Sof(H1SB)=Sof(H1SC)=1-FVAR(14)
 Sof(O2S)=Sof(C8S)=Sof(H8SA)=Sof(H8SB)=Sof(H8SC)=Sof(C7S)=Sof(H7SA)=Sof(H7SB)=
 Sof(C6S)=Sof(H6SA)=Sof(H6SB)=Sof(C5S)=Sof(H5SA)=Sof(H5SB)=Sof(H5SC)=Sof(O1S)=
 Sof(C4S)=Sof(H4SD)=Sof(H4SE)=Sof(H4SF)=Sof(C3S)=Sof(H3SC)=Sof(H3SD)=Sof(C2S)=
 Sof(H2SC)=Sof(H2SD)=Sof(C1S)=Sof(H1SD)=Sof(H1SE)=Sof(H1SF)=FVAR(14)
6.a Free rotating group:
 O2S(C8S,C7S,C6S,C5S), O2SA(C8SA,C7SA,C6SA,C5SA), O1SA(C4SA,C3SA,C2SA,C1SA),
 O1S(C4S,C3S,C2S,C1S)
6.b Secondary CH2 refined with riding coordinates:
 C7S(H7SA,H7SB), C6S(H6SA,H6SB), C7SA(H7SC,H7SD), C6SA(H6SC,H6SD), C3SA(H3SA,
 H3SB), C2SA(H2SA,H2SB), C3S(H3SC,H3SD), C2S(H2SC,H2SD)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C13(H13), C18(H18), C23(H23), C28(H28), C31(H31), C32(H32),
 C33(H33), C34(H34), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44),
  C45(H45), C46(H46), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55),
 C56(H56), C57(H57), C58(H58), C63(H63), C64(H64), C65(H65), C66(H66), C3'(H3'),
  C8'(H8'), C13'(H13'), C18'(H18'), C23'(H23'), C28'(H28'), C31'(H31'),
 C32'(H32'), C33'(H33'), C34'(H34'), C39'(H39'), C40'(H40'), C41'(H41'),
 C42'(H42'), C43'(H43'), C44'(H44'), C45'(H45'), C46'(H46'), C51'(H51'),
 C52'(H52'), C53'(H53'), C54'(H54'), C55'(H55'), C56'(H56'), C57'(H57'),
 C58'(H58'), C63'(H63'), C64'(H64'), C65'(H65'), C66'(H66')
6.d Idealised Me refined as rotating group:
 C8S(H8SA,H8SB,H8SC), C5S(H5SA,H5SB,H5SC), C8SA(H8SD,H8SE,H8SF), C5SA(H5SD,
 H5SE,H5SF), C4SA(H4SA,H4SB,H4SC), C1SA(H1SA,H1SB,H1SC), C4S(H4SD,H4SE,H4SF),
 C1S(H1SD,H1SE,H1SF)
;
_shelx_res_checksum              95785
_shelx_hkl_checksum              44936
_olex2_submission_special_instructions 'No special instructions were received'