Capture of Cesium Ions with Nanoclusters: Effects on Inter- and Intramolecular Assembly
Wei, Xiao; Kang, Xi; Yuan, Qianqin; Qin, Chenwanli; Jin, Shan; Wang, Shuxin; Zhu, Manzhou; Chemistry of Materials 31 (2019) 4945–; doi:10.1021/acs.chemmater.9b01890

data_4003008
_publ_section_title
;
 Capture of Cesium Ions with Nanoclusters: Effects on Inter- and
 Intramolecular Assembly
;
_journal_issue                   13
_journal_name_full               'Chemistry of Materials'
_journal_page_first              4945
_journal_paper_doi               10.1021/acs.chemmater.9b01890
_journal_volume                  31
_journal_year                    2019
_chemical_formula_moiety         'C89.5 H86.9 Ag29 Cs3 N5.75 O7 S24'
_chemical_formula_sum            'C89.5 H86.9 Ag29 Cs3 N5.75 O7 S24'
_chemical_formula_weight         5651.44
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.1264(11)
_cell_length_b                   27.9091(10)
_cell_length_c                   29.5657(12)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    160
_cell_measurement_theta_max      28.746
_cell_measurement_theta_min      2.219
_cell_volume                     28984.6(18)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      160
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            80120
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.459
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.945
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1148 before and 0.0531 after correction. The Ratio of minimum to maximum transmission is 0.7446. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.590
_exptl_crystal_description       block
_exptl_crystal_F_000             21057
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.809
_refine_diff_density_min         -3.079
_refine_diff_density_rms         0.255
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1738
_refine_ls_number_reflns         28264
_refine_ls_number_restraints     939
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0777P)^2^+117.0155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1427
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21142
_reflns_number_total             28264
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm9b01890_si_002.cif
_cod_data_source_block           20190109b_0ma
_cod_original_formula_sum        'C89.50 H86.90 Ag29 Cs3 N5.75 O7 S24'
_cod_database_code               4003008
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.638
_shelx_estimated_absorpt_t_min   0.638
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O03U-C74
 1.2 with sigma of 0.01
 O03U-C76
 1.2 with sigma of 0.01
 O032-C1AA = O032-C4
 1.2 with sigma of 0.01
 O16-C27
 1.2 with sigma of 0.01
 O16-N4
 2.5 with sigma of 0.02
 O1-C30
 1.2 with sigma of 0.01
 N2-C33 = N2-C5
 1.45 with sigma of 0.01
 C33-C5
 2.5 with sigma of 0.01
 Cs2-O6
 3 with sigma of 0.01
 O6-C2
 1.2 with sigma of 0.01
 N2-C2 = N2-C33 = N2-C5
 1.45 with sigma of 0.01
 C2-C5
 2.5 with sigma of 0.01
 C5-C33
 2.5 with sigma of 0.01
 C33-C2
 2.5 with sigma of 0.01
 Cs3-O1AA = Cs4A-O1AA
 3 with sigma of 0.01
 O1A-C30A
 1.2 with sigma of 0.01
 Cs3-O1AA = Cs3-O1AB = Cs4A-O1AA = Cs4-O1AB
 3 with sigma of 0.01
 O03U-N19
 2.5 with sigma of 0.01
 N34-C74 = N34-C49 = N34-C2AA
 1.45 with sigma of 0.01
 C74-C49
 2.5 with sigma of 0.01
 C74-C2AA
 2.5 with sigma of 0.01
 C2AA-C49
 2.5 with sigma of 0.01
 N19-C76 = N19-C65 = N19-C62
 1.45 with sigma of 0.01
 C62-C76
 2.5 with sigma of 0.01
 C62-C65
 2.5 with sigma of 0.01
 C65-C76
 2.5 with sigma of 0.01
 N14-C9 = N14-C8 = N14-C34
 1.45 with sigma of 0.01
 C9-C8
 2.5 with sigma of 0.01
 C8-C34
 2.5 with sigma of 0.01
 C34-C9
 2.5 with sigma of 0.01
 N03I-C1AA = N03J-C4 = N03J-C22 = N03I-C80 = N03J-C13 = N03I-C52
 1.45 with sigma of 0.01
 C1AA-C80
 2.5 with sigma of 0.01
 C80-C52
 2.5 with sigma of 0.01
 C52-C1AA
 2.5 with sigma of 0.01
 C4-C22
 2.5 with sigma of 0.01
 C22-C13
 2.5 with sigma of 0.01
 C13-C4
 2.5 with sigma of 0.01
 N0AA-C20 = N0AA-C51 = N0AA-C21
 1.45 with sigma of 0.01
 C51-C20
 2.5 with sigma of 0.01
 C51-C21
 2.5 with sigma of 0.01
 C21-C20
 2.5 with sigma of 0.01
 N4-C27 = N4-C3AA = N4-C31
 1.45 with sigma of 0.01
 C27-C3AA
 2.5 with sigma of 0.01
 C3AA-C31
 2.5 with sigma of 0.01
 C31-C27
 2.5 with sigma of 0.01
 N1AA-C30 = N1AA-C6 = N1AA-C10
 1.45 with sigma of 0.01
 C6-C30
 2.5 with sigma of 0.01
 C30-C10
 2.5 with sigma of 0.01
 C10-C6
 2.5 with sigma of 0.01
 N1AB-C30A = N1AB-C6A = N1AB-C10A
 1.45 with sigma of 0.01
 C6A-C10A
 2.5 with sigma of 0.01
 C10A-C30A
 2.5 with sigma of 0.01
 C30A-C6A
 2.5 with sigma of 0.01
 Cs2-O03F \\sim Cs2-O03G
 with sigma of 0.02
 N14-C9 \\sim N14A-C9A
 with sigma of 0.02
 C9-O03F \\sim C9A-O03G
 with sigma of 0.02
 Cs1-N14 \\sim Cs1-N14A
 with sigma of 0.04
 Cs1-C9 \\sim Cs1-C9A
 with sigma of 0.04
 Cs1-O03F \\sim Cs1-O03G
 with sigma of 0.04
 Cs2-C9 \\sim Cs2-C9A
 with sigma of 0.04
 N14-O03F \\sim N14A-O03G
 with sigma of 0.04
 C8-N14 \\sim C8A-N14A
 with sigma of 0.02
 N14-C34 \\sim N14A-C34A
 with sigma of 0.02
 C8-C9 \\sim C8A-C9A
 with sigma of 0.04
 C8-C34 \\sim C8A-C34A
 with sigma of 0.04
 C9-C34 \\sim C9A-C34A
 with sigma of 0.04
3. Restrained planarity
 C2AA, C49, C74, N34, O03U
 with sigma of 0.1
 C62, C65, C76, N19, O03U
 with sigma of 0.1
 C1AA, C52, C80, N03I
 with sigma of 0.1
 C1AA, C52, C80, N03I, O032
 with sigma of 0.1
 C4, C13, C22, N03J, O032
 with sigma of 0.1
 C20, C21, C51, N0AA, O0AA
 with sigma of 0.1
 C8A, C9A, C34A, N14A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C2 \\sim C5 \\sim C33 \\sim N2 \\sim O6: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C01X \\sim C02J \\sim C02V \\sim C03A \\sim C03F \\sim C4AA: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002
Cs3 \\sim Cs4 \\sim Cs4A: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
Cs3 \\sim Cs4 \\sim Cs4A \\sim O1AA \\sim O1AB: within 2A with sigma of 0.001
and sigma for terminal atoms of 0.002
Cs1 \\sim Cs2: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
Cs1 \\sim O03F: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C6 \\sim C10 \\sim C30 \\sim N1AA \\sim O1: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C02C \\sim C02M \\sim C03P \\sim C03Q \\sim C7 \\sim C022: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C0AA \\sim C01M \\sim C01R \\sim C01U \\sim C03B \\sim C030: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C30A \\sim N1AB \\sim C10A \\sim C6A: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002
Uanis(O6) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C33) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(Cs4A) \\sim Ueq, Uanis(Cs4) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O1AA) \\sim Ueq, Uanis(O1AB) \\sim Ueq: with sigma of 0.0001 and sigma
for terminal atoms of 0.0002
Uanis(O03F) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(C9) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(N14)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O03U) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(N19)
\\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(N34) \\sim Ueq,
Uanis(C49) \\sim Ueq, Uanis(C2AA) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O0AA) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(N0AA) \\sim Ueq, Uanis(C21)
\\sim Ueq, Uanis(C51) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O16) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C31)
\\sim Ueq, Uanis(C3AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(O1A) \\sim Ueq, Uanis(C30A) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(N1AA) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(N1AB) \\sim Ueq,
Uanis(C6A) \\sim Ueq, Uanis(C10A) \\sim Ueq, Uanis(C10) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9) \\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C8)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O03G) \\sim Ueq, Uanis(O03F) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C9A)
\\sim Ueq, Uanis(N14A) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C34A) \\sim Ueq,
Uanis(C8) \\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C1AA) \\sim Ueq, Uanis(N03I) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C80)
\\sim Ueq, Uanis(O032) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(N03J) \\sim Ueq,
Uanis(C13) \\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O18) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O1AA) = Uanis(O1AB)
5. Rigid body (RIGU) restrains
 C2, C5, C33, N2, O6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1AA, O1AB
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0002
 C8, C9, C34, N14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2AA, C49, C62, C65, C74, C76, N19, N34, O03U
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C20, C21, C51, N0AA, O0AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3AA, C27, C31, N4, O16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C6A, C10, C10A, C30, C30A, N1AA, N1AB, O1, O1A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C8, C8A, C9, C9A, C34, C34A, N14, N14A, O03F, O03G
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1AA, C4, C13, C22, C52, C80, N03I, N03J
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C16, C19, C47, N7, O18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Fixed Sof: C1AA(0.5) H1AA(0.5) C2(0.5) C2AA(0.25) H2AA(0.25) H2AB(0.25)
 H2AC(0.25) C02J(0.5) C3AA(0.5) H3AA(0.5) H3AB(0.5) H3AC(0.5) C4(0.5) C5(0.5)
 C6(0.35) H6A(0.35) H6B(0.35) H6C(0.35) C6A(0.15) H6AA(0.15) H6AB(0.15)
 H6AC(0.15) C8(0.55) H8A(0.55) H8B(0.55) H8C(0.55) C8A(0.45) H8AA(0.45)
 H8AB(0.45) H8AC(0.45) C9(0.55) H9(0.55) C9A(0.45) H9A(0.45) C10(0.35)
 H10A(0.35) H10B(0.35) H10C(0.35) C10A(0.15) H10D(0.15) H10E(0.15) H10F(0.15)
 C13(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C16(0.5) H16A(0.5) H16B(0.5) H16C(0.5)
 C19(0.5) H19A(0.85) H19B(0.85) H19C(0.85) C20(0.5) H20(0.5) C21(0.5) H21A(0.5)
 H21B(0.5) H21C(0.5) C22(0.5) H22A(0.5) H22B(0.5) H22C(0.5) C27(0.5) H27(0.5)
 C30(0.35) H30(0.35) C30A(0.15) H30A(0.15) C31(0.5) H31A(0.5) H31B(0.5)
 H31C(0.5) C33(0.5) C34(0.55) H34A(0.55) H34B(0.55) H34C(0.55) C34A(0.45)
 H34D(0.45) H34E(0.45) H34F(0.45) C47(0.5) H47(0.35) C49(0.25) H49A(0.25)
 H49B(0.25) H49C(0.25) C51(0.5) H51A(0.5) H51B(0.5) H51C(0.5) C52(0.5)
 H52A(0.5) H52B(0.5) H52C(0.5) C62(0.25) H62A(0.25) H62B(0.25) H62C(0.25)
 C65(0.25) H65A(0.25) H65B(0.25) H65C(0.25) C74(0.25) H74(0.25) C76(0.25)
 H76(0.25) C80(0.5) H80A(0.5) H80B(0.5) H80C(0.5) Cs3(0.5) Cs4(0.15) Cs4A(0.35)
 N0AA(0.5) N1AA(0.35) N1AB(0.15) N2(0.25) N03I(0.5) N03J(0.5) N4(0.5) N7(0.5)
 N14(0.55) N14A(0.45) N19(0.25) N34(0.25) O0AA(0.5) O1(0.35) O1A(0.15)
 O1AA(0.7) O1AB(0.3) O03F(0.55) O03G(0.45) O03U(0.5) O6(0.5) O16(0.5) O18(0.5)
7.a Riding coordinates:
 C47(H47)
7.b Ternary CH refined with riding coordinates:
 C1AA(H1AA), C9(H9), C9A(H9A), C20(H20)
7.c Me refined with riding coordinates:
 C2AA(H2AA,H2AB,H2AC), C3AA(H3AA,H3AB,H3AC), C6(H6A,H6B,H6C), C6A(H6AA,H6AB,
 H6AC), C8(H8A,H8B,H8C), C8A(H8AA,H8AB,H8AC), C10(H10A,H10B,H10C), C10A(H10D,
 H10E,H10F), C13(H13A,H13B,H13C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C),
 C31(H31A,H31B,H31C), C34(H34A,H34B,H34C), C34A(H34D,H34E,H34F), C49(H49A,H49B,
 H49C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C62(H62A,H62B,H62C), C65(H65A,
 H65B,H65C), C80(H80A,H80B,H80C)
7.d Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C01M(H01M), C01P(H01P), C01S(H01S), C01T(H01T), C01W(H01W),
 C02C(H02C), C02E(H02E), C02F(H02F), C02H(H02H), C02I(H02I), C4AA(H4AA),
 C03A(H03A), C03F(H03F), C02V(H02V), C02L(H02L), C02P(H02P), C02Q(H02Q),
 C02S(H02S), C02X(H02X), C02Y(H02Y), C02Z(H02Z), C03B(H03B), C03C(H03C),
 C03D(H03D), C03G(H03G), C03H(H03H), C03J(H03J), C03K(H03K), C03M(H03M),
 C03N(H03N), C03O(H03O), C03P(H03P), C03Q(H03Q), C7(H7), C021(H021), C024(H024),
  C025(H025), C27(H27), C028(H028), C029(H029), C30(H30), C030(H030),
 C30A(H30A), C031(H031), C033(H033), C034(H034), C035(H035), C036(H036),
 C037(H037), C038(H038), C039(H039), C74(H74), C76(H76)
7.e Fitted hexagon refined as free rotating group:
 C02J(C4AA,C01X,C03A,C03F,C02V)
7.f Idealised Me refined as rotating group:
 C03R(H03E,H03I,H03L), C03T(H03R,H03S,H03T), C16(H16A,H16B,H16C), C19(H19A,
 H19B,H19C)
;
_shelx_res_checksum              96141
_shelx_hkl_checksum              65785
_olex2_submission_special_instructions 'No special instructions were received'