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_7716113
_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_formula_moiety         'C31 H46 N2'
_chemical_formula_sum            'C31 H46 N2'
_chemical_formula_weight         446.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-14
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-04-30 deposited with the CCDC.	2024-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.311(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.8308(4)
_cell_length_b                   16.5393(4)
_cell_length_c                   21.5528(6)
_cell_measurement_reflns_used    17928
_cell_measurement_temperature    173
_cell_measurement_theta_max      23.7860
_cell_measurement_theta_min      1.5900
_cell_volume                     5641.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_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      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 0.889
_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    -75.00  83.00   0.50   45.00    --    4.40  45.00  60.00  316
  2  \w    -58.00 -33.00   0.50   45.00    --    4.40  45.00 179.95   50
  3  \w    -56.00 -30.00   0.50   45.00    --  -10.90  45.00 170.17   52
  4  \w     22.00  78.00   0.50   45.00    --  -10.90  45.00 -15.06  112
  5  \w    -94.00 -44.00   0.50   45.00    --  -10.90  45.00  90.00  100
  6  \w     -5.00  29.00   0.50   45.00    --  -10.90  45.00  90.00   68
  7  \w    -82.00 -56.00   0.50   45.00    --  -10.90  45.00  38.09   52
  8  \w     51.00  77.00   0.50   45.00    --  -10.90  45.00  90.00   52
  9  \w    -11.00  78.00   0.50   45.00    --  -10.90  45.00  38.09  178
 10  \w   -100.00 -73.00   0.50   45.00    --  -10.90  45.00 170.17   54
 11  \w   -100.00  61.00   0.50   45.00    --  -10.90  45.00 120.00  322
 12  \w   -100.00  78.00   0.50   45.00    --  -10.90  45.00 175.68  356
;
_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      0.0074710000
_diffrn_orient_matrix_UB_12      0.0418153000
_diffrn_orient_matrix_UB_13      0.0049954000
_diffrn_orient_matrix_UB_21      -0.0361048000
_diffrn_orient_matrix_UB_22      0.0020792000
_diffrn_orient_matrix_UB_23      0.0188251000
_diffrn_orient_matrix_UB_31      0.0254735000
_diffrn_orient_matrix_UB_32      -0.0093158000
_diffrn_orient_matrix_UB_33      0.0265360000
_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  0.0622
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.889
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            121505
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.440
_diffrn_reflns_theta_min         1.552
_diffrn_source                   'Rotating Anode'
_diffrn_source_type              'Rigaku FR-X'
_exptl_absorpt_coefficient_mu    0.060
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.74a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.052
_exptl_crystal_description       prism
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         13897
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1449
_refine_ls_R_factor_gt           0.0759
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0870P)^2^+2.1682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1686
_refine_ls_wR_factor_ref         0.1962
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8174
_reflns_number_total             13897
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01298d2.cif
_cod_data_source_block           cbas72
_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               7716113
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-H1 = N41-H41
 0.98 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C52) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C58) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H58C)=Sof(H58D)=Sof(C59B)=Sof(H59D)=Sof(H59E)=Sof(H59F)=1-FVAR(1)
 Sof(H58A)=Sof(H58B)=Sof(C59A)=Sof(H59A)=Sof(H59B)=Sof(H59C)=FVAR(1)
 Sof(H52A)=Sof(C54B)=Sof(H54D)=Sof(H54E)=Sof(H54F)=Sof(C53A)=Sof(H53D)=
 Sof(H53E)=Sof(H53F)=1-FVAR(2)
 Sof(H52)=Sof(C53B)=Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(C54A)=Sof(H54A)=
 Sof(H54B)=Sof(H54C)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C31(H31), C71(H71), C28(H28), C55(H55), C12(H12), C68(H68), C52(H52),
 C52(H52A), C15(H15)
5.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C60(H60A,H60B), C58(H58A,H58B), C58(H58C,H58D), C18(H18A,H18B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C43(H43), C24(H24), C26(H26), C25(H25), C8(H8), C65(H65), C66(H66),
 C64(H64), C50(H50), C10(H10), C49(H49), C9(H9), C48(H48)
5.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C33(H33A,H33B,H33C), C21(H21A,H21B,H21C), C32(H32A,H32B,
 H32C), C17(H17A,H17B,H17C), C73(H73A,H73B,H73C), C56(H56A,H56B,H56C), C14(H14A,
 H14B,H14C), C13(H13A,H13B,H13C), C61(H61A,H61B,H61C), C57(H57A,H57B,H57C),
 C29(H29A,H29B,H29C), C72(H72A,H72B,H72C), C30(H30A,H30B,H30C), C16(H16A,H16B,
 H16C), C69(H69A,H69B,H69C), C59A(H59A,H59B,H59C), C70(H70A,H70B,H70C),
 C53B(H53A,H53B,H53C), C54A(H54A,H54B,H54C), C59B(H59D,H59E,H59F), C54B(H54D,
 H54E,H54F), C53A(H53D,H53E,H53F)
;
_shelx_res_checksum              75319