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_7714030
_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         'C29 H41 Cs N2'
_chemical_formula_sum            'C29 H41 Cs N2'
_chemical_formula_weight         550.55
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-01-09
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.7640(3)
_cell_length_b                   10.7073(2)
_cell_length_c                   12.7363(2)
_cell_measurement_reflns_used    9565
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      31.37
_cell_measurement_theta_min      2.73
_cell_volume                     2831.62(8)
_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  'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_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 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  0.0365
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            105261
_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         31.538
_diffrn_reflns_theta_min         2.485
_exptl_absorpt_coefficient_mu    1.325
_exptl_absorpt_correction_T_max  0.1199
_exptl_absorpt_correction_T_min  0.0743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1320 before and 0.0599 after correction.
The Ratio of minimum to maximum transmission is 0.6197.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_description       needle
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 3724 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         9463
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0250
_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^)+(0.0243P)^2^+0.8804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0579
_reflns_Friedel_coverage         0.923
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                8561
_reflns_number_total             9463
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01592k2.cif
_cod_data_source_block           155am22hv849nacnaccs_0ma
_cod_database_code               7714030
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.708
_shelx_estimated_absorpt_t_min   0.633
_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.a Ternary CH refined with riding coordinates:
 C24(H24), C27(H27), C12(H12), C15(H15)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C20(H20), C21(H21), C22(H22), C8(H8), C9(H9), C10(H10)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C),
 C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C14(H14A,H14B,H14C), C13(H13A,H13B,
 H13C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              52523
_shelx_hkl_checksum              89893
_olex2_submission_special_instructions 'No special instructions were received'