Revealing unbound β-diketiminate anions: structural dynamics from caesium complexes.
Videa, Hellen; Martínez-Martínez, Antonio J; Dalton transactions (Cambridge, England : 2003) 52 (2023) 13058–13062; doi:10.1039/d3dt01592k

data_7714032
_publ_section_title
;
 Revealing unbound &#x3b2;-diketiminate anions: structural dynamics from
 caesium complexes.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13058
_journal_page_last               13062
_journal_paper_doi               10.1039/d3dt01592k
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C24 H48 Cs O12, C29 H41 N2'
_chemical_formula_sum            'C53 H89 Cs N2 O12'
_chemical_formula_weight         1079.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-10
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-04-17 deposited with the CCDC.	2023-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.4710(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.0601(5)
_cell_length_b                   13.0041(2)
_cell_length_c                   18.7072(3)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      41.14
_cell_measurement_theta_min      2.82
_cell_volume                     5624.82(17)
_computing_cell_refinement       'Bruker Apex3, 2020'
_computing_data_collection       'Bruker Apex3, 2020'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker D8 Quest'
_diffrn_measurement_device_type  'Bruker CHi Fixed Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            222006
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         41.176
_diffrn_reflns_theta_min         2.694
_diffrn_source                   'microfocus sealed x-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I/mS high brilliance'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_T_max  0.1610
_exptl_absorpt_correction_T_min  0.1067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0864 before and 0.0405 after correction.
The Ratio of minimum to maximum transmission is 0.6627.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       plate
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.330
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     936
_refine_ls_number_reflns         36941
_refine_ls_number_restraints     4732
_refine_ls_restrained_S_all      1.192
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0283
_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^)+(0.0344P)^2^+3.2146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0771
_reflns_Friedel_coverage         0.977
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                30397
_reflns_number_total             36941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01592k2.cif
_cod_data_source_block           186am22vgr07cs216c6_100k_0ma
_cod_database_code               7714032
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.882
_shelx_estimated_absorpt_t_min   0.847
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.49(3)
 0.51(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O2-C34 = O2-C1F = O3-C37 = O3-C33 = O4-C30 = O5-C1A = O6-C1C = O6-C1B = O7-C1E
 1.43 with sigma of 0.02
 O6-C1B = O6-C1C = O6A-C1Y = O6A-C1S = O7-C1D = O7-C1E = O7A-C1T = O7A-C1Z =
 O2-C1F = O2-C34 = O2A-C1R = O2A-C34A = O3-C37 = O3-C33 = O3A-C37A = O3A-C33A =
 O4-C30 = O4-C38 = O4A-C30A = O4A-C38A = O5-C35 = O5-C1A = O5A-C35A = O5A-C1Q
 1.42 with sigma of 0.01
 C37-C34 = C1R-C1Z = C1F-C1E = C1S-C1T = C1D-C1C = C1Q-C1Y = C1B-C1A = C38A-
 C35A = C38-C35 = C33A-C30A = C33-C30 = C37A-C34A
 1.49 with sigma of 0.01
 C1I-C1H = C1V-C1W = C31-C1G = C39-C36 = C39A-C36A = C32-C1O = C32A-C2A = C1M-
 C1L = C1K-C1J = C40-C1X
 1.49 with sigma of 0.01
 O13-C32 = O13-C1M = O13A-C32A = O11-C1L = O11-C1K = O11A-C1N = O11A-C40 = O10-
 C1J = O10-C1I = O10A-C1X = O10A-C1W = O9-C1H = O9-C1G = O9A-C1V = O8-C31 = O8-
 C36 = O8A-C31A = O8A-C36A = O1-C1O = O1A-C39A = O1A-C2A
 1.42 with sigma of 0.1
 O4-C38 = O7-C1D
 1.42 with sigma of 0.02
 C41-C1N
 1.49 with sigma of 0.01
 O11A-C41
 1.42 with sigma of 0.01
 C34-C37 = C33-C30 = C1A-C1B = C1C-C1D = C1E-C1F
 1.49 with sigma of 0.02
 C42-C31A
 1.49 with sigma of 0.01
 O8A-C42
 1.42 with sigma of 0.01
 C33-Cs1
 4.2 with sigma of 0.01
 C37A-C34A
 1.49 with sigma of 0.01
 O9-C1H
 1.42 with sigma of 0.02
 C39-C36 = C31-C1G = C1H-C1I = C1J-C1K = C1L-C1M
 1.49 with sigma of 0.02
 C33-C30
 1.4 with sigma of 0.1
 O3-C33
 1.42 with sigma of 0.1
 O1-C39 = O1-C1O = O8-C36 = O8-C31 = O9-C1G = O10-C1I = O10-C1J = O11-C1L =
 O11-C1K
 1.43 with sigma of 0.02
 C1M-C1L = C1O-C32
 1.49 with sigma of 0.01
 O13-C32 = O13-C1M
 1.43 with sigma of 0.01
 O3-C37
 1.42 with sigma of 0.1
 O4-C33 = O5-C1B
 2.38 with sigma of 0.04
 C33A-C37A
 2.38 with sigma of 0.01
 C1S-C1Y
 2.38 with sigma of 0.01
 C41-C40
 2.38 with sigma of 0.01
 C32A-C1N
 2.38 with sigma of 0.01
 C42-C36A
 2.38 with sigma of 0.01
 O2-C37 = O2-C1E = O3-C34 = O3-C30 = O5-C38 = O6-C1D = O7-C1F = O7-C1C
 2.37 with sigma of 0.04
 O6-C1A
 2.36 with sigma of 0.04
 O7A-C1R = O2A-C37A
 2.4 with sigma of 0.01
 C1R-C34A
 2.38 with sigma of 0.01
 C37A-C33A
 2.38 with sigma of 0.01
 O11-C1J
 2.36 with sigma of 0.04
 C37-C33
 2.38 with sigma of 0.01
 C33-O4
 2.38 with sigma of 0.01
 O1-C36 = O8-C39 = O8-C1G = O10-C1H = O11-C1M
 2.37 with sigma of 0.04
 O9-C31 = O9-C1I = O10-C1K
 2.38 with sigma of 0.04
 O2-C34 \\sim O2-C1F \\sim O3-C37 \\sim O3-C33 \\sim O4-C30 \\sim O4-C38 \\sim
O5-C1A \\sim O6-C1B \\sim O6-
 C1C \\sim O7-C1D \\sim O7-C1E
 with sigma of 0.02
 C34-C37 \\sim C33-C30 \\sim C1A-C1B \\sim C1C-C1D \\sim C1E-C1F
 with sigma of 0.02
 C37-C33 \\sim C30-C38 \\sim C1B-C1C \\sim C1D-C1E \\sim C1F-C34
 with sigma of 0.04
 O2-C37 \\sim O3-C30 \\sim O5-C1B \\sim O6-C1D \\sim O7-C1F \\sim O3-C34 \\sim
O4-C33 \\sim O5-C38 \\sim O6-
 C1A \\sim O7-C1C \\sim O2-C1E
 with sigma of 0.04
 C39-C36 \\sim C31-C1G \\sim C1H-C1I \\sim C1J-C1K \\sim C1L-C1M
 with sigma of 0.02
 O1-C39 \\sim O1-C1O \\sim O8-C36 \\sim O8-C31 \\sim O9-C1G \\sim O9-C1H \\sim
O10-C1I \\sim O10-C1J \\sim O11-
 C1K \\sim O11-C1L
 with sigma of 0.02
 C36-C31 \\sim C1G-C1H \\sim C1I-C1J \\sim C1K-C1L \\sim C1O-C39
 with sigma of 0.04
 O1-C36 \\sim O8-C1G \\sim O9-C1I \\sim O10-C1K \\sim O11-C1M \\sim O8-C39
\\sim O9-C31 \\sim O10-C1H ~
 O11-C1J
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim C34 \\sim C37 \\sim C33
\\sim C30 \\sim C38 \\sim C1A \\sim C1B \\sim C1C \\sim C1D \\sim C1E \\sim
C1F: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
O1 \\sim O8 \\sim O9 \\sim O10 \\sim O11 \\sim C39 \\sim C36 \\sim C31 \\sim
C1G \\sim C1H \\sim C1I \\sim C1J \\sim C1K \\sim C1L \\sim C1M \\sim C1O:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Cs1 \\sim O4A \\sim O5 \\sim O13 \\sim O11 \\sim O11A \\sim O8A \\sim O3A \\sim
O2 \\sim O6A \\sim O9 \\sim O13A \\sim O4 \\sim C38A \\sim C30A \\sim C35 \\sim
C1A \\sim C1M \\sim C32 \\sim O6 \\sim O5A \\sim C1B \\sim H1BA \\sim C35A
\\sim H35C \\sim C1Q \\sim H1QB \\sim C1K \\sim C1L \\sim C40 \\sim C41 \\sim
C1O \\sim H1OB \\sim O1 \\sim C39A \\sim H39D \\sim C36A \\sim C39 \\sim H39B
\\sim C1I \\sim H1IA \\sim C1J \\sim H1JB \\sim O10A \\sim O10 \\sim C1X \\sim
H1XB \\sim C42 \\sim C33A \\sim C37A \\sim C34 \\sim C1F \\sim C1S \\sim C1Y
\\sim H32B \\sim O1A \\sim C2A \\sim H2AA \\sim C37 \\sim H37A \\sim O2A \\sim
C34A \\sim H34D \\sim C1R \\sim H1RB \\sim C1G \\sim C1H \\sim O3 \\sim C33
\\sim H33B \\sim C1N \\sim C32A \\sim C30 \\sim C38 \\sim H38C \\sim H38D \\sim
H30C \\sim H30D \\sim H35A \\sim H35B \\sim H1AA \\sim H1AB \\sim H1MA \\sim
H1MB \\sim H32A \\sim C1C \\sim H1BB \\sim H35D \\sim H1QA \\sim H1KA \\sim
H1KB \\sim H1LA \\sim H1LB \\sim H40A \\sim H40B \\sim H41A \\sim H41B \\sim
H1OA \\sim H39C \\sim H36C \\sim H36D \\sim H39A \\sim C36 \\sim H1IB \\sim
H1JA \\sim C1W \\sim H1XA \\sim C31A \\sim H42A \\sim H42B \\sim H33C \\sim
H33D \\sim H37C \\sim H37D \\sim H34A \\sim H34B \\sim C1E \\sim H1FA \\sim
H1FB \\sim H1SA \\sim H1SB \\sim C1T \\sim H1YA \\sim H1YB \\sim H2AB \\sim
H37B \\sim H34C \\sim H1RA \\sim C1Z \\sim C31 \\sim H1GA \\sim H1GB \\sim H1HA
\\sim H1HB \\sim C1V \\sim H1WA \\sim H33A \\sim H1NA \\sim H1NB \\sim H32C
\\sim H32D \\sim H30A \\sim H30B \\sim H38A \\sim H38B \\sim H1CA \\sim H1CB
\\sim C1D \\sim O8 \\sim H36A \\sim H36B \\sim H1WB \\sim O9A \\sim H31C \\sim
H31D \\sim O7 \\sim H1EA \\sim H1EB \\sim O7A \\sim H1TA \\sim H1TB \\sim H1ZA
\\sim H1ZB \\sim H31A \\sim H31B \\sim H1VA \\sim H1VB \\sim H1DA \\sim H1DB:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(O3) = Uanis(O3A)
Uanis(C33A) = Uanis(C30)
5. Rigid body (RIGU) restrains
 O2, O3, O4, O5, O6, O7, C34, C37, C33, C30, C38, C1A, C1B, C1C, C1D, C1E, C1F
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, O8, O9, O10, O11, C39, C36, C31, C1G, C1H, C1I, C1J, C1K, C1L, C1M, C1O
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cs1, O4A, O5, O13, O11, O11A, O8A, O3A, O2, O6A, O9, O13A, O4, C38A, C30A,
 C35, C1A, C1M, C32, O6, O5A, C1B, H1BA, C35A, H35C, C1Q, H1QB, C1K, C1L, C40,
 C41, C1O, H1OB, O1, C39A, H39D, C36A, C39, H39B, C1I, H1IA, C1J, H1JB, O10A,
 O10, C1X, H1XB, C42, C33A, C37A, C34, C1F, C1S, C1Y, H32B, O1A, C2A, H2AA, C37,
  H37A, O2A, C34A, H34D, C1R, H1RB, C1G, C1H, O3, C33, H33B, C1N, C32A, C30,
 C38, H38C, H38D, H30C, H30D, H35A, H35B, H1AA, H1AB, H1MA, H1MB, H32A, C1C,
 H1BB, H35D, H1QA, H1KA, H1KB, H1LA, H1LB, H40A, H40B, H41A, H41B, H1OA, H39C,
 H36C, H36D, H39A, C36, H1IB, H1JA, C1W, H1XA, C31A, H42A, H42B, H33C, H33D,
 H37C, H37D, H34A, H34B, C1E, H1FA, H1FB, H1SA, H1SB, C1T, H1YA, H1YB, H2AB,
 H37B, H34C, H1RA, C1Z, C31, H1GA, H1GB, H1HA, H1HB, C1V, H1WA, H33A, H1NA,
 H1NB, H32C, H32D, H30A, H30B, H38A, H38B, H1CA, H1CB, C1D, O8, H36A, H36B,
 H1WB, O9A, H31C, H31D, O7, H1EA, H1EB, O7A, H1TA, H1TB, H1ZA, H1ZB, H31A, H31B,
  H1VA, H1VB, H1DA, H1DB
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C35(0.5) H35A(0.5) H35B(0.5) O2(0.5) O3(0.5) O4(0.5) O5(0.5)
 O6(0.5) O7(0.5) C34(0.5) H34A(0.5) H34B(0.5) C37(0.5) H37A(0.5) H37B(0.5)
 C33(0.5) H33A(0.5) H33B(0.5) C30(0.5) H30A(0.5) H30B(0.5) C38(0.5) H38A(0.5)
 H38B(0.5) C1A(0.5) H1AA(0.5) H1AB(0.5) C1B(0.5) H1BA(0.5) H1BB(0.5) C1C(0.5)
 H1CA(0.5) H1CB(0.5) C1D(0.5) H1DA(0.5) H1DB(0.5) C1E(0.5) H1EA(0.5) H1EB(0.5)
 C1F(0.5) H1FA(0.5) H1FB(0.5) O1(0.5) O8(0.5) O9(0.5) O10(0.5) O11(0.5)
 C39(0.5) H39A(0.5) H39B(0.5) C36(0.5) H36A(0.5) H36B(0.5) C31(0.5) H31A(0.5)
 H31B(0.5) C1G(0.5) H1GA(0.5) H1GB(0.5) C1H(0.5) H1HA(0.5) H1HB(0.5) C1I(0.5)
 H1IA(0.5) H1IB(0.5) C1J(0.5) H1JA(0.5) H1JB(0.5) C1K(0.5) H1KA(0.5) H1KB(0.5)
 C1L(0.5) H1LA(0.5) H1LB(0.5) C1M(0.5) H1MA(0.5) H1MB(0.5) C1O(0.5) H1OA(0.5)
 H1OB(0.5) O13(0.5) C32(0.5) H32A(0.5) H32B(0.5) O11A(0.5) O13A(0.5) O5A(0.5)
 O2A(0.5) O9A(0.5) O10A(0.5) O4A(0.5) O8A(0.5) O7A(0.5) O3A(0.5) O1A(0.5)
 O6A(0.5) C38A(0.5) H38C(0.5) H38D(0.5) C35A(0.5) H35C(0.5) H35D(0.5) C40(0.5)
 H40A(0.5) H40B(0.5) C1N(0.5) H1NA(0.5) H1NB(0.5) C32A(0.5) H32C(0.5) H32D(0.5)
 C1Q(0.5) H1QA(0.5) H1QB(0.5) C33A(0.5) H33C(0.5) H33D(0.5) C30A(0.5) H30C(0.5)
 H30D(0.5) C34A(0.5) H34C(0.5) H34D(0.5) C1R(0.5) H1RA(0.5) H1RB(0.5) C39A(0.5)
 H39C(0.5) H39D(0.5) C36A(0.5) H36C(0.5) H36D(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5)
 C1T(0.5) H1TA(0.5) H1TB(0.5) C1V(0.5) H1VA(0.5) H1VB(0.5) C1W(0.5) H1WA(0.5)
 H1WB(0.5) C1X(0.5) H1XA(0.5) H1XB(0.5) C31A(0.5) H31C(0.5) H31D(0.5) C1Y(0.5)
 H1YA(0.5) H1YB(0.5) C1Z(0.5) H1ZA(0.5) H1ZB(0.5) C2A(0.5) H2AA(0.5) H2AB(0.5)
 C37A(0.5) H37C(0.5) H37D(0.5) C41(0.5) H41A(0.5) H41B(0.5) C42(0.5) H42A(0.5)
 H42B(0.5)
7.a Ternary CH refined with riding coordinates:
 C27(H27), C15(H15), C24(H24), C12(H12)
7.b Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C34(H34A,H34B), C37(H37A,H37B), C33(H33A,H33B), C30(H30A,
 H30B), C38(H38A,H38B), C1A(H1AA,H1AB), C1B(H1BA,H1BB), C1C(H1CA,H1CB),
 C1D(H1DA,H1DB), C1E(H1EA,H1EB), C1F(H1FA,H1FB), C39(H39A,H39B), C36(H36A,H36B),
  C31(H31A,H31B), C1G(H1GA,H1GB), C1H(H1HA,H1HB), C1I(H1IA,H1IB), C1J(H1JA,
 H1JB), C1K(H1KA,H1KB), C1L(H1LA,H1LB), C1M(H1MA,H1MB), C1O(H1OA,H1OB),
 C32(H32A,H32B), C38A(H38C,H38D), C35A(H35C,H35D), C40(H40A,H40B), C1N(H1NA,
 H1NB), C32A(H32C,H32D), C1Q(H1QA,H1QB), C33A(H33C,H33D), C30A(H30C,H30D),
 C34A(H34C,H34D), C1R(H1RA,H1RB), C39A(H39C,H39D), C36A(H36C,H36D), C1S(H1SA,
 H1SB), C1T(H1TA,H1TB), C1V(H1VA,H1VB), C1W(H1WA,H1WB), C1X(H1XA,H1XB),
 C31A(H31C,H31D), C1Y(H1YA,H1YB), C1Z(H1ZA,H1ZB), C2A(H2AA,H2AB), C37A(H37C,
 H37D), C41(H41A,H41B), C42(H42A,H42B)
7.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C3(H3), C21(H21), C10(H10), C20(H20), C9(H9), C8(H8)
7.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C14(H14A,H14B,H14C), C26(H26A,H26B,H26C), C25(H25A,H25B,
 H25C), C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C17(H17A,H17B,H17C), C16(H16A,H16B,
 H16C), C29(H29A,H29B,H29C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              2691
_shelx_hkl_checksum              51255
_olex2_submission_special_instructions 'No special instructions were received'