Design of Pure Heterodinuclear Lanthanoid Cryptate Complexes
Buch, Christian Dirk; Hansen, Steen H.; Mitcov, Dmitri; Tram, Camilla Mia; Nichol, Gary Stephen; Brechin, Euan K.; Piligkos, Stergios; Chemical Science  (2021) –; doi:10.1039/D1SC00987G

data_1561833
_publ_section_title
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 Design of Pure Heterodinuclear Lanthanoid Cryptate Complexes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC00987G
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C39 H45 N10 O9 Y2, N O3, 2.5(H2 O), 1.5[H2O]'
_chemical_formula_sum            'C39 H53 N11 O16 Y2'
_chemical_formula_weight         1109.74
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc2747rd
_audit_creation_date             2021-01-29
_audit_creation_method
;
Olex2 1.3-beta
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-01-29 deposited with the CCDC.	2021-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.6029(6)
_cell_length_b                   17.6029(6)
_cell_length_c                   29.0488(15)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.550
_cell_measurement_theta_min      2.401
_cell_volume                     9001.1(6)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0932
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            126935
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.818
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.650
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1086 before and 0.0825 after correction.
The Ratio of minimum to maximum transmission is 0.6882.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_description       needle
_exptl_crystal_F_000             4560
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.114
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 2703 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.034(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         7955
_refine_ls_number_restraints     127
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0370P)^2^+10.1103P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0835
_reflns_Friedel_coverage         0.755
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                6911
_reflns_number_total             7955
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc00987g2.cif
_cod_data_source_block           mo_d8v4644_0m_a
_cod_original_cell_volume        9001.1(8)
_cod_database_code               1561833
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.752
_shelx_estimated_absorpt_t_min   0.449
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O13-H13B = O13-H13A = O13A-H13C = O13A-H13D = O16-H16D = O16-H16E = O14-H14A
 0.84 with sigma of 0.02
 O15-H15
 0.84 with sigma of 0.02
 H16E-H16D_$1 = H14A_$1-H14A
 1.35 with sigma of 0.04
 H13B-H13A = H13C-H13D = H16D-H16E
 1.35 with sigma of 0.04
 H15_$2-H15
 1.35 with sigma of 0.04
 O12A-N11A \\sim O11A-N11A \\sim O10A-N11A \\sim O10-N11 \\sim O11-N11 \\sim
O12-N11
 with sigma of 0.02
 N9-O4A \\sim N9-O4 \\sim N9-O5 \\sim N9-O6
 with sigma of 0.02
3. Restrained planarity
 O4A, O5, O6, N9
 with sigma of 0.1
 O4, O5, O6, N9
 with sigma of 0.1
4. Rigid body (RIGU) restrains
 O10, O11, O12, N11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10A, O11A, O12A, N11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4, O5, O6, N9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4A, O5, O6, N9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O7, O8, O9, N10} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O10, O11, O12, N11}
{O7, O8, O9, N10} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O10A, O11A, O12A, N11A}
6. Others
 Sof(O4A)=1-FVAR(1)
 Sof(O4)=FVAR(1)
 Fixed Sof: O10(0.5) O11(0.5) O12(0.5) N11(0.5) O10A(0.5) O11A(0.5) O12A(0.5)
 N11A(0.5) O13(0.5) H13A(0.5) H13B(0.5) O13A(0.5) H13C(0.5) H13D(0.5) H16D(0.5)
7.a Everything fixed:
 O13, H13A, H13B, O13A, H13C, H13D, O14, H14A, O16, H16D, H16E
7.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,
 H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C9(H9), C12(H12), C14(H14), C17(H17), C18(H18),
 C21(H21), C23(H23), C26(H26), C27(H27)
7.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C16(H16A,H16B,H16C), C25(H25A,H25B,H25C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              22565
_shelx_hkl_checksum              67077
_shelx_fab_checksum              33897
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 800'
_olex2_submission_original_sample_id D8V4644
_olex2_submission_special_instructions 'No special instructions were received'