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_7714031
_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, C7 H8'
_chemical_formula_sum            'C60 H97 Cs N2 O12'
_chemical_formula_weight         1171.30
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-10
_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                77.660(3)
_cell_angle_beta                 77.052(2)
_cell_angle_gamma                73.081(2)
_cell_formula_units_Z            2
_cell_length_a                   13.7097(6)
_cell_length_b                   15.1667(7)
_cell_length_c                   16.4016(8)
_cell_measurement_reflns_used    9844
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      26.82
_cell_measurement_theta_min      2.38
_cell_volume                     3139.2(3)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'Bruker D8 Quest'
_diffrn_measurement_device_type  'Bruker CHi Fixed Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0781
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            101941
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.101
_diffrn_reflns_theta_min         2.204
_exptl_absorpt_coefficient_mu    0.647
_exptl_absorpt_correction_T_max  0.1375
_exptl_absorpt_correction_T_min  0.0913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1110 before and 0.0836 after correction.
The Ratio of minimum to maximum transmission is 0.6640.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       block
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.106
_refine_diff_density_min         -1.334
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         15060
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0651P)^2^+2.5520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1142
_refine_ls_wR_factor_ref         0.1279
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12113
_reflns_number_total             15060
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01592k2.cif
_cod_data_source_block           113am21hv652_0m
_cod_database_code               7714031
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.892
_olex2_refinement_description
;
1. 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
2. Restrained distances
 O10-C48A \\sim O10-C48 \\sim O11-C49A \\sim O11-C49
 with sigma of 0.01
 C49A-C48A \\sim C49-C48
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C48 \\sim C49 \\sim C48A \\sim C49A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 C48, C49, C48A, C49A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C48A)=Sof(H48C)=Sof(H48D)=Sof(C49A)=Sof(H49C)=Sof(H49D)=1-FVAR(1)
 Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C49)=Sof(H49A)=Sof(H49B)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27)
6.b Secondary CH2 refined with riding coordinates:
 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), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B),
  C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C50(H50A,
 H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C48(H48A,H48B),
 C49(H49A,H49B), C48A(H48C,H48D), C49A(H49C,H49D)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C55(H55),
 C56(H56), C57(H57), C58(H58), C59(H59)
6.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C60(H60A,H60B,H60C)
;
_shelx_res_checksum              38399
_shelx_hkl_checksum              85292
_olex2_submission_special_instructions 'No special instructions were received'