Synthesis, stereocontrol and structural studies of highly luminescent chiral tris-amidepyridyl-triazacyclononane lanthanide complexes.
Neil, Emily R.; Funk, Alexander M.; Yufit, Dmitry S.; Parker, David; Dalton transactions (Cambridge, England : 2003) 43 (2014) 5490–5504; doi:10.1039/c3dt53000k

data_7029543
_publ_section_title
;
 Synthesis, stereocontrol and structural studies of highly luminescent
 chiral tris-amidepyridyl-triazacyclononane lanthanide complexes.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5490
_journal_page_last               5504
_journal_paper_doi               10.1039/c3dt53000k
_journal_volume                  43
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C51 H57 N9 O3 Yb1, 3(C F3 O3 S)'
_chemical_formula_sum            'C54 H57 F9 N9 O12 S3 Yb'
_chemical_formula_weight         1464.30
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3'
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-02-14
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   21.836(2)
_cell_length_b                   21.836(2)
_cell_length_c                   11.1868(17)
_cell_measurement_reflns_used    5425
_cell_measurement_temperature    120
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     4619.4(9)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART v5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XH, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      120
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\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  0.0398
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            65596
_diffrn_reflns_theta_full        28.98
_diffrn_reflns_theta_max         31.03
_diffrn_reflns_theta_min         1.08
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.75
_diffrn_source_target            Mo
_diffrn_source_type              'sealed X-ray tube'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.713
_exptl_absorpt_correction_T_max  0.7769
_exptl_absorpt_correction_T_min  0.1508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2006/1 (Bruker,2006) was used for absorption correction.
R(int) was 0.0847 before and 0.0366 after correction.
The Ratio of minimum to maximum transmission is 0.1941.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shard
_exptl_crystal_F_000             2217
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.197
_refine_diff_density_min         -1.011
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.018(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         5472
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+9.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1123
_reflns_number_gt                5432
_reflns_number_total             5472
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53000k2.cif
_cod_data_source_block           S_[YbL1]_13srv030
_cod_original_cell_volume        4619.5(10)
_cod_database_code               7029543
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H16 of C16, H15 of C15, H14 of C14, H13 of C13, H12 of C12, H10 of C10,
  {H3A,H3B} of C3, {H2A,H2B} of C2, H7 of C7, H6 of C6, H5 of C5, {H1A,H1B} of
  C1, H3 of N3
 At 1.5 times of:
  {H17A,H17B,H17C} of C17
2. Restrained distances
 S1B-O2 \~ S1A-O2 \~ S1B-O4B \~ S1A-O4A \~ S1A-O3A \~ S1B-O3B
 with sigma of 0.01
 S1B-C1SB \~ S1A-C1SA
 with sigma of 0.01
 F3A-C1SB \~ F3B-C1SA \~ F2A-C1SB \~ F2B-C1SA \~ F1B-C1SB \~ F1A-C1SA
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uiso(F1B) = Uiso(F1A) = Uiso(F2A) = Uiso(F2B) = Uiso(F3B) = Uiso(F3A)
Uiso(O4A) = Uiso(O3B) = Uiso(O3A) = Uiso(O4B)
4. Others
 Fixed Sof: S1B(0.5) F1B(0.5) F2B(0.5) F3B(0.5) O3B(0.5) O4B(0.5) C1SB(0.5)
 O4A(0.5) O3A(0.5) S1A(0.5) C1SA(0.5) F3A(0.5) F2A(0.5) F1A(0.5)
5.a Ternary CH refined with riding coordinates:
 C10(H10)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B)
5.c Aromatic/amide H refined with riding coordinates:
 N3(H3), C5(H5), C6(H6), C7(H7), C12(H12), C13(H13), C14(H14), C15(H15),
 C16(H16)
5.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C)
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