Functionalized Triptycene-Derived Tripodal Ligands: Privileged Formation of Tetranuclear Cage Assemblies with Larger Ln(III)
Vuillamy, Alexandra; Zebret, Soumaila; Besnard, Céline; Placide, Virginie; Petoud, Stéphane; Hamacek, Josef; Inorganic Chemistry  (2017) –; doi:10.1021/acs.inorgchem.6b02900

data_4345226
_publ_section_title
;
 Functionalized Triptycene-Derived Tripodal Ligands: Privileged Formation
 of Tetranuclear Cage Assemblies with Larger Ln(III)
;
_journal_name_full               'Inorganic Chemistry'
_journal_paper_doi               10.1021/acs.inorgchem.6b02900
_journal_year                    2017
_chemical_formula_moiety         'C188 H158 Eu4 N24 O51, 10(Cl O4), 3(C2 H3 N)'
_chemical_formula_sum            'C194 H167 Cl10 Eu4 N27 O91'
_chemical_formula_weight         5294.88
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-26
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.07.25 svn.r3318 for OlexSys, GUI svn.r5204)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.8968(3)
_cell_length_b                   37.8968(3)
_cell_length_c                   37.8968(3)
_cell_measurement_reflns_used    14699
_cell_measurement_temperature    180
_cell_measurement_theta_max      39.9663
_cell_measurement_theta_min      2.6177
_cell_volume                     54426.2(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      180
_diffrn_detector_area_resol_mean 10.4679
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_details
;
  1 omega  -65.00   28.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.5615   38.0000 -150.0000 186

  2 omega -115.00  -83.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.5615 -138.0000 -148.0000 64

  3 omega   61.00   87.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       37.5615 -138.0000   86.0000 52

  4 omega   37.00   72.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -45.0000  120.0000 70
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.940
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            66892
_diffrn_reflns_point_group_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        67.680
_diffrn_reflns_theta_max         73.254
_diffrn_reflns_theta_min         2.607
_exptl_absorpt_coefficient_mu    8.118
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66145
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             21360
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1066
_refine_ls_number_reflns         16789
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1308
_refine_ls_R_factor_gt           0.0909
_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^)+(0.0861P)^2^+289.1515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2181
_refine_ls_wR_factor_ref         0.2487
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10775
_reflns_number_total             16789
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02900_si_002.cif
_cod_data_source_block           sousept2
_cod_original_cell_volume        54426.2(13)
_cod_database_code               4345226
_shelx_estimated_absorpt_t_max   0.923
_shelx_estimated_absorpt_t_min   0.294
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 Cl2-O2E \\sim Cl2-O1E \\sim Cl2-O4E \\sim Cl2-O3E
 with sigma of 0.02
 O1E-O4E \\sim O1E-O2E \\sim O1E-O3E \\sim O2E-O3E \\sim O2E-O4E \\sim O3E-O4E
 with sigma of 0.02
 Cl2-O1F \\sim Cl2-O4F \\sim Cl2-O3F \\sim Cl2-O2F
 with sigma of 0.02
 O1F-O2F \\sim O1F-O3F \\sim O1F-O4F \\sim O2F-O3F \\sim O2F-O4F \\sim O3F-O4F
 with sigma of 0.02
 Cl1G-O3G \\sim Cl1G-O4G \\sim Cl1G-O2G \\sim Cl1G-O1G
 with sigma of 0.02
 Cl1H-O4H \\sim Cl1H-O1H \\sim Cl1H-O2H \\sim Cl1H-O3H
 with sigma of 0.02
 O1H-O2H \\sim O1H-O3H \\sim O1H-O4H \\sim O2H-O3H \\sim O2H-O4H \\sim O3H-O4H
 with sigma of 0.04
 Cl1G-O3G \\sim Cl1G-O1G \\sim Cl1G-O2G \\sim Cl1G-O4G
 with sigma of 0.02
 O1G-O2G \\sim O1G-O3G \\sim O1G-O4G \\sim O2G-O3G \\sim O2G-O4G \\sim O3G-O4G
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(O3G) = Uanis(O4H)
4. Rigid body (RIGU) restrains
 O2E, O3E, O4E, O1E, Cl2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2F, O4F, O3F, O1F, Cl2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1G, Cl1G, O4G, O2G, O3G
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1H, Cl1H, O4H, O2H, O3H
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O2F)=Sof(O4F)=Sof(O3F)=Sof(O1F)=1-FVAR(1)
 Sof(O2E)=Sof(O3E)=Sof(O4E)=Sof(O1E)=FVAR(1)
 Sof(Cl1H)=Sof(O4H)=Sof(O2H)=Sof(O1H)=Sof(O3H)=1-FVAR(2)
 Sof(O3G)=Sof(Cl1G)=Sof(O4G)=Sof(O1G)=Sof(O2G)=FVAR(2)
6.a Rotating group:
 OW(HWA,HWB)
6.b Ternary CH refined with riding coordinates:
 C2(H2), C2D(H2D), C1(H1), C1D(H1DA)
6.c Aromatic/amide H refined with riding coordinates:
 C5A(H5A), C13D(H13D), C11D(H11D), C5D(H5D), N1A(H1A), N1B(H1B), C8C(H8C),
 C13A(H13A), N1D(H1D), C8D(H8D), C8B(H8B), C4C(H4C), N1C(H1C), C11B(H11B),
 C5B(H5B), C6D(H6D), C11C(H11C), C5C(H5C), C6B(H6B), C11A(H11A), C8A(H8A),
 C13B(H13B), C6A(H6A), C13C(H13C)
6.d Idealised Me refined as rotating group:
 C17D(H17A,H17B,H17C), C23C(H23A,H23B,H23C), C17C(H17D,H17E,H17F), C17B(H17G,
 H17H,H17I), C17A(H17J,H17K,H17L), C23A(H23D,H23E,H23F), C23B(H23G,H23H,H23I),
 C23D(H23J,H23K,H23L), C9(H9A,H9B,H9C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'