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_7711715
_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         'C35 H33 F7 N7 O7 Yb, 4.2(H2 O), 0.4(H O)'
_chemical_formula_sum            'C35 H41.8 F7 N7 O11.6 Yb'
_chemical_formula_weight         1052.19
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-07-07
_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                90
_cell_angle_beta                 113.294(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0200(14)
_cell_length_b                   22.477(2)
_cell_length_c                   14.9599(16)
_cell_measurement_reflns_used    9858
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      30.62
_cell_measurement_theta_min      2.34
_cell_volume                     4021.2(7)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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  0.0975
_diffrn_reflns_av_unetI/netI     0.0649
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            88634
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.711
_diffrn_reflns_theta_min         1.703
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.427
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1483 before and 0.0697 after correction. The Ratio of minimum to maximum transmission is 0.6054. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_description       plate
_exptl_crystal_F_000             2106
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.082
_refine_diff_density_max         2.137
_refine_diff_density_min         -1.535
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         12433
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0374P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0824
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8768
_reflns_number_total             12433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02266d2.cif
_cod_data_source_block           eb2004
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C35 H41.80 F7 N7 O11.60 Yb'
_cod_database_code               7711715
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.826
_shelx_estimated_absorpt_t_min   0.365
_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, All O(H,H) groups, All O(H,H,H,H,H) groups, All O(H,H,
  H,H,H,H) groups
2. Restrained distances
 O3SA-H3SA
 0.95 with sigma of 0.02
 O4SA-H4SC
 0.95 with sigma of 0.02
 O1S-H1SA
 0.95 with sigma of 0.02
 O2S-H2SA
 0.95 with sigma of 0.02
 O3SB-H3SD
 0.95 with sigma of 0.02
 O3SB-H3SC
 0.95 with sigma of 0.02
 H3SD-H3SC
 1.35 with sigma of 0.02
 O1S-H1SB
 0.95 with sigma of 0.02
 O4SB-H4SB
 1 with sigma of 0.02
 O5SA-H4SB
 1 with sigma of 0.02
 H3SB-O3SA
 0.95 with sigma of 0.02
 O2S-H2SB
 0.95 with sigma of 0.02
 O5SB-H5SB
 0.95 with sigma of 0.02
 O4SA-H4SD
 0.95 with sigma of 0.02
 O5SA-H5SA
 0.95 with sigma of 0.02
 O4SB-H4SA
 0.95 with sigma of 0.02
 H5SA-H4SB
 1.5 with sigma of 0.02
 H4SB-H4SA
 1.5 with sigma of 0.02
 H1SA-H1SB
 1.5 with sigma of 0.02
 H2SA-H2SB
 1.5 with sigma of 0.02
 H3SC-H3SD
 1.5 with sigma of 0.02
 H3SA-H3SB
 1.5 with sigma of 0.02
 O5SA-H4SB \\sim O4SB-H4SB
 with sigma of 0.02
 F2-C10 \\sim O1S-H1SA \\sim O1T-H1SA
 with sigma of 0.02
 O1T-H1SB \\sim O1S-H1SB
 with sigma of 0.02
3. Others
 Fixed Sof: O3SA(0.5) O2S(0.6) O1S(0.6) O4SA(0.6) O4SB(0.6) O5SB(0.4)
 O5SA(0.4) H3SA(0.5) H4SC(0.6) O3SB(0.5) H3SC(0.5) H2SA(0.6) H3SD(0.5) O1T(0.4)
 H3SB(0.5) H2SB(0.6) H5SB(0.4) H4SD(0.6) H5SA(0.4) H4SA(0.6)
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C21(H21A,H21B), C2(H2A,H2B), C3(H3A,H3B), C12(H12A,H12B),
 C13(H13A,H13B), C1(H1A,H1B), C23(H23A,H23B), C34(H34A,H34B), C22(H22A,H22B)
4.b Aromatic/amide H refined with riding coordinates:
 N6(H6), N7(H7), C7(H7A), C17(H17), C26(H26), C5(H5), C33(H33), C27(H27),
 C30(H30), C15(H15)
4.c Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C)
;
_shelx_res_checksum              56544
_shelx_hkl_checksum              20060
_olex2_submission_special_instructions 'No special instructions were received'