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_7714033
_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         'C18 H36 Cs N2 O6, C29 H41 N2'
_chemical_formula_sum            'C47 H77 Cs N4 O6'
_chemical_formula_weight         927.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 95.5900(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4068(6)
_cell_length_b                   15.8513(5)
_cell_length_c                   19.0928(8)
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      29.474
_cell_measurement_theta_min      2.498
_cell_volume                     4941.8(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker Apex3, 2020'
_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  '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 0.999
_diffrn_measurement_device       'Bruker D8 Quest'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_unetI/netI     0.0163
_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       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            483098
_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         29.628
_diffrn_reflns_theta_min         2.495
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.797
_exptl_absorpt_correction_T_max  0.1402
_exptl_absorpt_correction_T_min  0.1073
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1263 before and 0.0622 after correction.
The Ratio of minimum to maximum transmission is 0.7653.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       plate
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         13922
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0238P)^2^+3.4140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0725
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12548
_reflns_number_total             13922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01592k2.cif
_cod_data_source_block           184am22hvcscrypt_0m
_cod_database_code               7714033
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.870
_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
 C27-C29 \\sim C27-C29A
 with sigma of 0.02
 C27-C28 \\sim C27-C28A
 with sigma of 0.02
 C28-C27 \\sim C28A-C27 \\sim C29-C27 \\sim C29A-C27
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C27 \\sim C29 \\sim C28 \\sim C28A \\sim C29A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Uanis(C28) = Uanis(C28A)
Uanis(C29A) = Uanis(C29)
4. Rigid body (RIGU) restrains
 C27, C29, C28, C28A, C29A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H27A)=Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29A)=Sof(H29D)=
 Sof(H29E)=Sof(H29F)=1-FVAR(1)
 Sof(H27)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C28)=Sof(H28A)=Sof(H28B)=
 Sof(H28C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C15(H15), C24(H24), C12(H12), C27(H27), C27(H27A)
6.b Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C41(H41A,H41B), C45(H45A,H45B), C32(H32A,H32B), C36(H36A,
 H36B), C46(H46A,H46B), C39(H39A,H39B), C47(H47A,H47B), C31(H31A,H31B),
 C37(H37A,H37B), C42(H42A,H42B), C43(H43A,H43B), C33(H33A,H33B), C35(H35A,H35B),
  C38(H38A,H38B), C34(H34A,H34B), C44(H44A,H44B), C30(H30A,H30B)
6.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C21(H21), C9(H9), C20(H20), C3(H3), C8(H8), C22(H22)
6.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C14(H14A,H14B,H14C), C5(H5A,H5B,H5C), C17(H17A,H17B,H17C),
 C16(H16A,H16B,H16C), C13(H13A,H13B,H13C), C26(H26A,H26B,H26C), C25(H25A,H25B,
 H25C), C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C28A(H28D,H28E,H28F),
 C29A(H29D,H29E,H29F)
;
_shelx_res_checksum              20657
_shelx_hkl_checksum              98025
_olex2_submission_special_instructions 'No special instructions were received'