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_1561840
_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 Gd N10 O9 Y, N O3, 2.5(H2 O), 1[H2O]'
_chemical_formula_sum            'C39 H52 Gd N11 O15.5 Y'
_chemical_formula_weight         1169.07
_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
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2747qc
_audit_creation_date             2021-02-03
_audit_creation_method
;
Olex2 1.3-beta
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-02-03 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                   17.6312(4)
_cell_length_b                   17.6312(4)
_cell_length_c                   29.2044(12)
_cell_measurement_reflns_used    9195
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.224
_cell_measurement_theta_min      2.390
_cell_volume                     9078.5(5)
_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 2014/5 (Sheldrick, 2014)'
_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  0.0524
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            118541
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         1.811
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.802
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1416 before and 0.0728 after correction.
The Ratio of minimum to maximum transmission is 0.6938.
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    1.711
_exptl_crystal_description       rod
_exptl_crystal_F_000             4720
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 3994 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.021(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         10414
_refine_ls_number_restraints     127
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+13.6477P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0693
_reflns_Friedel_coverage         0.773
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                9540
_reflns_number_total             10414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc00987g2.cif
_cod_data_source_block           mo_d8v4647_0m_a
_cod_original_cell_volume        9078.5(6)
_cod_original_formula_sum        'C39 H52 Gd N11 O15.50 Y'
_cod_database_code               1561840
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.759
_shelx_estimated_absorpt_t_min   0.187
_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. Shared sites
{Gd1, Y1A}
{Y2, Gd2A}
3. Restrained distances
 O16-H16D = O16-H16E = O14-H14A = O15_$1-H15_$6 = O13A-H13C = O13A-H13D = O13-
 H13A = O13-H13B
 0.84 with sigma of 0.02
 H16E-H16D_$7 = H14A_$7-H14A = H15_$2-H15_$3
 1.35 with sigma of 0.04
 H13B-H13A = H13C-H13D = H16E_$4-H16D_$5
 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
4. Restrained planarity
 N9, O4A, O6, O5
 with sigma of 0.1
 N9, O4, O5, O6
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(Gd1) = Uanis(Y1A)
Uanis(Y2) = Uanis(Gd2A)
6. 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
 N9, O4, O5, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4A, N9, O5, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. 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}
8. Others
 Sof(Y1A)=Sof(Gd2A)=1-FVAR(1)
 Sof(Gd1)=Sof(Y2)=FVAR(1)
 Sof(O4A)=1-FVAR(2)
 Sof(O4)=FVAR(2)
 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)
9.a Everything fixed:
 O13, H13A, H13B, O13A, H13C, H13D, O14, H14A, O15, H15, O16, H16D, H16E
9.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)
9.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)
9.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              51907
_shelx_hkl_checksum              77075
_shelx_fab_checksum              58956
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 800'
_olex2_submission_original_sample_id D8V4647
_olex2_submission_special_instructions 'No special instructions were received'