Design and synthesis of covalently tethered “isoG-star” as a recyclable host for selective cesium separation
Liu, Mengjia; He, Ying; Wojtas, Lukasz; Shi, Xiaodong; Green Chemistry 25 (2023) 8494–8499; doi:10.1039/D3GC02932H

data_7247480
_publ_section_title
;
 Design and synthesis of covalently tethered &#x201C;isoG-star&#x201D; as
 a recyclable host for selective cesium separation
;
_journal_issue                   21
_journal_name_full               'Green Chemistry'
_journal_page_first              8494
_journal_page_last               8499
_journal_paper_doi               10.1039/D3GC02932H
_journal_volume                  25
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C31 H43 N5 O7 Si, 1.052(C1 H4 O1), 0.185(H2 O1), 0.293(O1.5)'
_chemical_formula_sum            'C32.05 H47.58 N5 O8.68 Si'
_chemical_formula_weight         669.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-05-16
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-06 deposited with the CCDC.	2023-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.985(2)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   44.2430(10)
_cell_length_b                   19.9018(6)
_cell_length_c                   17.7791(6)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      77.96
_cell_measurement_theta_min      2.46
_cell_volume                     14616.5(8)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Bruker PHOTON II CMOS area detector'
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture Single Source'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_unetI/netI     0.0559
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            102233
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.802
_diffrn_reflns_theta_min         2.464
_diffrn_source                   'Microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec ImuS'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.027
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.6109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1372 before and 0.0770 after correction.
The Ratio of minimum to maximum transmission is 0.8099.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       plate
_exptl_crystal_F_000             5733
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 7884 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.030(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1838
_refine_ls_number_reflns         29057
_refine_ls_number_restraints     462
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0569
_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^)+(0.0975P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.1661
_reflns_Friedel_coverage         0.831
_reflns_Friedel_fraction_full    0.955
_reflns_Friedel_fraction_max     0.853
_reflns_number_gt                21250
_reflns_number_total             29057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3gc02932h2.cif
_cod_data_source_block           626
_cod_depositor_comments
'Adding full bibliography for 7247479--7247480.cif.'
_cod_original_cell_volume        14616.4(8)
_cod_database_code               7247480
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.853
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups,
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O71G-C72G = O71I-C72I = O71J-C72J = O71K-C72K = O71H-C72H
 1.4 with sigma of 0.02
 O71L-H71A = O71L-H71B
 0.9 with sigma of 0.02
 O31B-H71A = O71H_$1-H71B
 2 with sigma of 0.02
 H71A-H71B
 1.4 with sigma of 0.04
 O38C-C39E \\sim O38C-C39C
 with sigma of 0.01
 C46E-C45C \\sim C46C-C45C
 with sigma of 0.01
 C40D-C39D \\sim C40F-C39D
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O43B \\sim C44B \\sim C45B \\sim C46B \\sim C47B: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
O38C \\sim C39C \\sim C40C \\sim C41C \\sim C42C \\sim C39E \\sim C40E \\sim
C41E \\sim C42E: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C44C \\sim C45C \\sim C46C \\sim C47C \\sim C46E \\sim C47E: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C39D \\sim C40D \\sim C41D \\sim C42D \\sim C40F \\sim C41F \\sim C42F: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 O43B, C44B, C45B, C46B, C47B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O38C, C39C, C40C, C41C, C42C, C39E, C40E, C41E, C42E
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C44C, C45C, C46C, C47C, C46E, C47E
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C39D, C40D, C41D, C42D, C40F, C41F, C42F
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{C39A, C40A, C41A, C42A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C44B, C45B, C46B, C47B}
{C40A, C41A, C42A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C40D, C41D, C42D}
{C41A, C42A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C46E, C47E}
{C40A, C41A, C42A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C40F, C41F, C42F}
{C41A, C42A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C46C, C47C}
{C39A, C40A, C41A, C42A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C39E, C40E, C41E, C42E}
{C39A, C40A, C41A, C42A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C39C, C40C, C41C, C42C}
6. Others
 Sof(H45C)=Sof(H45D)=Sof(C46E)=Sof(H46E)=Sof(C47E)=Sof(H47C)=Sof(H47D)=1-FVAR(1)
 Sof(H45A)=Sof(H45B)=Sof(C46C)=Sof(H46C)=Sof(C47C)=Sof(H47A)=Sof(H47B)=FVAR(1)
 Sof(C39E)=Sof(H39C)=Sof(H39D)=Sof(C40E)=Sof(H40C)=Sof(H40D)=Sof(C41E)=
 Sof(H41E)=Sof(C42E)=Sof(H42C)=Sof(H42D)=1-FVAR(2)
 Sof(C39C)=Sof(H39A)=Sof(H39B)=Sof(C40C)=Sof(H40A)=Sof(H40B)=Sof(C41C)=
 Sof(H41C)=Sof(C42C)=Sof(H42A)=Sof(H42B)=FVAR(2)
 Sof(O71G)=Sof(H71G)=Sof(C72G)=Sof(H72A)=Sof(H72B)=Sof(H72C)=FVAR(3)
 Sof(O71I)=Sof(H71I)=Sof(C72I)=Sof(H72G)=Sof(H72H)=Sof(H72I)=FVAR(4)
 Sof(O73J)=1-FVAR(5)
 Sof(O71J)=Sof(H71J)=Sof(C72J)=Sof(H72J)=Sof(H72K)=Sof(H72L)=FVAR(5)
 Sof(H39G)=Sof(H39H)=Sof(C40F)=Sof(H40G)=Sof(H40H)=Sof(C41F)=Sof(H41F)=
 Sof(C42F)=Sof(H42G)=Sof(H42H)=1-FVAR(6)
 Sof(H39E)=Sof(H39F)=Sof(C40D)=Sof(H40E)=Sof(H40F)=Sof(C41D)=Sof(H41D)=
 Sof(C42D)=Sof(H42E)=Sof(H42F)=FVAR(6)
 Sof(O71L)=Sof(H71A)=Sof(H71B)=FVAR(7)
 Fixed Sof: O81L(0.5) O82L(0.5) O83L(0.25) O84L(0.25)
7.a Ternary CH refined with riding coordinates:
 C18A(H18A), C20A(H20A), C21A(H21A), C18B(H18B), C20B(H20B), C21B(H21B),
 C18C(H18C), C20C(H20C), C21C(H21C), C18D(H18D), C20D(H20D), C21D(H21D)
7.b Secondary CH2 refined with riding coordinates:
 C22A(H22E,H22F), C28A(H28E,H28F), C39A(H39I,H39J), C40A(H40I,H40J), C44A(H44E,
 H44F), C45A(H45G,H45H), C22B(H22G,H22H), C28B(H28G,H28H), C39B(H39K,H39L),
 C40B(H40K,H40L), C44B(H44G,H44H), C45B(H45I,H45J), C22C(H22A,H22B), C28C(H28A,
 H28B), C39C(H39A,H39B), C40C(H40A,H40B), C39E(H39C,H39D), C40E(H40C,H40D),
 C44C(H44A,H44B), C45C(H45A,H45B), C45C(H45C,H45D), C22D(H22C,H22D), C28D(H28C,
 H28D), C39D(H39E,H39F), C39D(H39G,H39H), C40D(H40E,H40F), C40F(H40G,H40H),
 C44D(H44C,H44D), C45D(H45E,H45F)
7.c Aromatic/amide H refined with riding coordinates:
 N3A(H3A), C9A(H9A), C33A(H33A), C35A(H35A), C37A(H37A), C41A(H41A),
 C46A(H46A), N3B(H3B), C9B(H9B), C33B(H33B), C35B(H35B), C37B(H37B), C41B(H41B),
  C46B(H46B), N3C(H3C), C9C(H9C), C33C(H33C), C35C(H35C), C37C(H37C),
 C41C(H41C), C41E(H41E), C46C(H46C), C46E(H46E), N5D(H5D), C9D(H9D), C33D(H33D),
  C35D(H35D), C37D(H37D), C41D(H41D), C41F(H41F), C46D(H46D)
7.d X=CH2 refined with riding coordinates:
 N1A(H1AA,H1AB), C42A(H42I,H42J), C47A(H47G,H47H), N1B(H1BA,H1BB), C42B(H42K,
 H42L), C47B(H47I,H47J), N1C(H1CA,H1CB), C42C(H42A,H42B), C42E(H42C,H42D),
 C47C(H47A,H47B), C47E(H47C,H47D), N1D(H1DA,H1DB), C42D(H42E,H42F), C42F(H42G,
 H42H), C47D(H47E,H47F)
7.e Idealised Me refined as rotating group:
 C51A(H51G,H51H,H51I), C52A(H52G,H52H,H52I), C54A(H54G,H54H,H54I), C55A(H55G,
 H55H,H55I), C56A(H56G,H56H,H56I), C51B(H51J,H51K,H51L), C52B(H52J,H52K,H52L),
 C54B(H54J,H54K,H54L), C55B(H55J,H55K,H55L), C56B(H56J,H56K,H56L), C51C(H51A,
 H51B,H51C), C52C(H52A,H52B,H52C), C54C(H54A,H54B,H54C), C55C(H55A,H55B,H55C),
 C56C(H56A,H56B,H56C), C51D(H51D,H51E,H51F), C52D(H52D,H52E,H52F), C54D(H54D,
 H54E,H54F), C55D(H55D,H55E,H55F), C56D(H56D,H56E,H56F), C72G(H72A,H72B,H72C),
 C72H(H72D,H72E,H72F), C72I(H72G,H72H,H72I), C72J(H72J,H72K,H72L), C72K(H72M,
 H72N,H72O)
7.f Idealised tetrahedral OH refined as rotating group:
 O71G(H71G), O71H(H71H), O71I(H71I), O71J(H71J), O71K(H71K)
;
_shelx_res_checksum              64906
_shelx_hkl_checksum              25351
_olex2_submission_special_instructions 'No special instructions were received'