Improved emission of Yb(III) ions in triazacyclononane-based macrocyclic ligands compared to cyclen-based ones.
Kiraev, Salauat R.; Mathieu, Emilie; Kovacs, Daniel; Wells, Jordann A. L.; Tomar, Monika; Andres, Julien; Borbas, K. Eszter; Dalton transactions (Cambridge, England : 2003) 51 (2022) 16596–16604; doi:10.1039/d2dt02266d

data_7711716
_publ_section_title
;
 Improved emission of Yb(III) ions in triazacyclononane-based macrocyclic
 ligands compared to cyclen-based ones.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16596
_journal_page_last               16604
_journal_paper_doi               10.1039/d2dt02266d
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety
'C33 H35 N7 O8 Yb, C33 H34 N7 O8 Yb, 2(Cl), 19(O)'
_chemical_formula_sum            'C66 H69 Cl2 N14 O35 Yb2'
_chemical_formula_weight         2035.33
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-07-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-07 deposited with the CCDC.	2022-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                87.265(2)
_cell_angle_beta                 77.2410(10)
_cell_angle_gamma                63.2700(10)
_cell_formula_units_Z            2
_cell_length_a                   16.0996(14)
_cell_length_b                   17.255(2)
_cell_length_c                   20.7070(18)
_cell_measurement_reflns_used    9608
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.62
_cell_measurement_theta_min      2.28
_cell_volume                     5002.0(8)
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      170.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            108311
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.677
_diffrn_reflns_theta_min         1.910
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.990
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1227 before and 0.0564 after correction. The Ratio of minimum to maximum transmission is 0.7604. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       plate
_exptl_crystal_F_000             2034
_exptl_crystal_size_max          0.636
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.126
_refine_diff_density_max         2.341
_refine_diff_density_min         -1.175
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1092
_refine_ls_number_reflns         30622
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0487P)^2^+7.1089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1007
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25003
_reflns_number_total             30622
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02266d2.cif
_cod_data_source_block           eb2005
_cod_original_cell_volume        5001.9(9)
_cod_database_code               7711716
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.788
_shelx_estimated_absorpt_t_min   0.364
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: Cl1(0.5) Cl2(0.5) Cl3(0.5) Cl4(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C65(H65A,H65B), C11(H11A,H11B), C32(H32A,H32B), C19(H19A,H19B),
 C20(H20A,H20B), C1(H1A,H1B), C21(H21A,H21B), C45(H45A,H45B), C12(H12A,H12B),
 C10(H10A,H10B), C53(H53A,H53B), C2(H2A,H2B), C52(H52A,H52B), C54(H54A,H54B),
 C36(H36A,H36B), C44(H44A,H44B), C35(H35A,H35B), C34(H34A,H34B), C43(H43A,H43B)
3.b Aromatic/amide H refined with riding coordinates:
 N14(H14A), N6(H6), N13(H13), N7(H7), C24(H24), C31(H31), C28(H28), C64(H64),
 C57(H57), C14(H14), C25(H25), C60(H60), C49(H49), C15(H15), C16(H16), C7(H7A),
 C5(H5), C48(H48), C47(H47), C6(H6A), C40(H40), C39(H39), C38(H38)
3.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C66(H66A,H66B,H66C)
;
_shelx_res_checksum              61880
_shelx_hkl_checksum              33475
_shelx_fab_checksum              25834
_olex2_submission_special_instructions 'No special instructions were received'