Alkyl backbone variations in common β-diketiminate ligands and applications to <i>N</i>-heterocyclic silylene chemistry.
Bourne, Connor; Dong, Huanhuan; McKain, Katharine; Mayer, Lena C.; McKay, Aidan P.; Cordes, David B.; Slawin, Alexandra M. Z.; Stasch, Andreas; Dalton transactions (Cambridge, England : 2003) 53 (2024) 9887–9895; doi:10.1039/d4dt01298d

data_7716115
_publ_section_title
;
 Alkyl backbone variations in common &#x3b2;-diketiminate ligands and
 applications to <i>N</i>-heterocyclic silylene chemistry.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9887
_journal_page_last               9895
_journal_paper_doi               10.1039/d4dt01298d
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C31 H44 N2 Si'
_chemical_formula_sum            'C31 H44 N2 Si'
_chemical_formula_weight         472.77
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-01
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-04-30 deposited with the CCDC.	2024-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   42.4215(8)
_cell_length_b                   15.2419(4)
_cell_length_c                   8.7768(2)
_cell_measurement_reflns_used    9300
_cell_measurement_temperature    173
_cell_measurement_theta_max      29.4180
_cell_measurement_theta_min      2.7090
_cell_volume                     5674.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'photon counting pixel array detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Dectris PILATUS P200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -85.00  91.70   0.38   12.00    --    4.40  45.00   0.00  465
  2  \w   -100.00  76.32   0.38   12.00    --  -11.10  45.00 150.00  464
  3  \w     52.00  77.08   0.38   12.00    --  -11.10  45.00  30.00   66
  4  \w    -15.00  48.08   0.38   12.00    --  -11.10  45.00  30.00  166
;
_diffrn_measurement_device       'AFC10: Fixed \c 3 circle'
_diffrn_measurement_device_type  'Rigaku XtaLAB P200K'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support Loop
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0005008500
_diffrn_orient_matrix_UB_12      -0.0222152500
_diffrn_orient_matrix_UB_13      -0.0709609000
_diffrn_orient_matrix_UB_21      -0.0166061000
_diffrn_orient_matrix_UB_22      0.0039220000
_diffrn_orient_matrix_UB_23      -0.0064338000
_diffrn_orient_matrix_UB_31      0.0018776500
_diffrn_orient_matrix_UB_32      0.0407098500
_diffrn_orient_matrix_UB_33      -0.0381191000
_diffrn_radiation_monochromator  'Rigaku Osmic Confocal Optical System'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.847
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            15725
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.847
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.625
_diffrn_reflns_theta_min         1.920
_diffrn_source                   'Rotating Anode'
_diffrn_source_type              'Rigaku FR-X'
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97040
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_description       prism
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.170
_refine_diff_density_min         -0.171
_refine_diff_density_rms         0.028
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.46(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2949
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0268
_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^)+(0.0421P)^2^+2.6487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0702
_reflns_Friedel_coverage         0.641
_reflns_Friedel_fraction_full    0.834
_reflns_Friedel_fraction_max     0.614
_reflns_number_gt                2857
_reflns_number_total             2949
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01298d2.cif
_cod_data_source_block           hdas65
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7716105--7716116.cif.
;
_cod_database_code               7716115
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.980
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.54(12)
 0.46(12)
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, All C(H,H,H,H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C16B) = Uanis(C16A)
4. Others
 Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(1)
 Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(1)
 Fixed Sof: C16A(0.5) H16A(0.5) H16B(0.5) C16B(0.5) H16C(0.5)
5.a Ternary CH refined with riding coordinates:
 C13(H13), C10(H10)
5.b Secondary CH2 refined with riding coordinates:
 C16A(H16A,H16B)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C3(H3), C8(H8), C7(H7), C16B(H16C)
5.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C17(H17D,H17E,H17F), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C15(H15A,H15B,H15C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              46280