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_7716116
_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 H45 K N2, C6 H6'
_chemical_formula_sum            'C37 H51 K N2'
_chemical_formula_weight         562.89
_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             2023-06-01
_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                 93.499(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5987(4)
_cell_length_b                   15.6955(5)
_cell_length_c                   18.1851(7)
_cell_measurement_reflns_used    10931
_cell_measurement_temperature    173
_cell_measurement_theta_max      66.2760
_cell_measurement_theta_min      3.6610
_cell_volume                     3304.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.82a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.82a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.82a (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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'hybrid photon counting detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Dectris PILATUS P100K'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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    -23.00  47.00   1.00    5.00    --    0.00 -82.00  90.00   70
  2  \w    -23.00  47.00   1.00    5.00    --    0.00 -82.00 -90.00   70
  3  \w    -15.00  35.00   1.00    5.00    --    5.00  77.00 150.00   50
  4  \w    -15.00  35.00   1.00    5.00    --    5.00  77.00  30.00   50
  5  \w    -15.00  35.00   1.00    5.00    --    5.00  77.00 -60.00   50
  6  \w   -141.00 -69.00   1.00   10.00    --  -57.40 -19.00-150.00   72
  7  \w    -60.00  32.00   1.00   10.00    --  -57.40  37.00  60.00   92
  8  \w   -141.00 -88.00   1.00   10.00    --  -57.40 -77.00  30.00   53
  9  \w   -141.00 -88.00   1.00   10.00    --  -57.40 -77.00 -60.00   53
 10  \w    -46.00  32.00   1.00   10.00    --  -57.40  19.00 150.00   78
 11  \w   -141.00 -69.00   1.00   10.00    --  -57.40 -19.00  30.00   72
 12  \w   -141.00 -88.00   1.00   10.00    --  -57.40 -77.00  90.00   53
 13  \w   -167.00 -45.00   1.00   25.00    --  -83.30 -70.00-163.19  122
 14  \w   -193.00 -77.00   1.00   40.00    -- -109.20 -57.00-106.04  116
 15  \w   -193.00 -71.00   1.00   40.00    -- -109.20 -70.00 -99.93  122
 16  \w    -97.00 -20.00   1.00   40.00    -- -109.20  82.00 -21.38   77
 17  \w   -193.00 -98.00   1.00   40.00    -- -109.20 -43.00 -41.32   95
 18  \w    -97.00 -20.00   1.00   40.00    -- -109.20  82.00  89.58   77
 19  \w   -193.00 -89.00   1.00   40.00    -- -109.20 -50.00 -90.66  104
 20  \w   -193.00-124.00   1.00   40.00    -- -109.20 -21.00 109.35   69
 21  \w    -93.00 -31.00   1.00   40.00    -- -109.20  82.00 -70.95   62
 22  \w   -193.00-158.00   1.00   40.00    -- -109.20 -60.00 -57.73   35
 23  \w   -131.00 -76.00   1.00   40.00    -- -109.20 -60.00 -57.73   55
 24  \w   -192.00-145.00   1.00   40.00    -- -109.20 -61.00  54.09   47
 25  \w   -120.00 -94.00   1.00   40.00    -- -109.20  67.00  92.22   26
 26  \w    -90.00 -61.00   1.00   40.00    -- -109.20  67.00  92.22   29
 27  \w   -166.00-140.00   1.00   40.00    -- -109.20 -19.00  90.00   26
 28  \w    -93.00 -55.00   1.00   40.00    -- -109.20  82.00 134.61   38
 29  \w   -130.00 -98.00   1.00   40.00    -- -109.20 -43.00 -16.86   32
 30  \w   -185.00-133.00   1.00   40.00    -- -109.20 -43.00 -16.86   52
 31  \w   -135.00 -98.00   1.00   40.00    -- -109.20 -44.00  41.39   37
 32  \w   -193.00-154.00   1.00   40.00    -- -109.20 -44.00  41.39   39
 33  \w   -111.00 -85.00   1.00   40.00    -- -109.20 -53.00  27.46   26
 34  \w    -73.00 -47.00   1.00   40.00    -- -109.20  19.00 150.00   26
;
_diffrn_measurement_device       'AFC12: Kappa 4 circle'
_diffrn_measurement_device_type  'Rigaku XtaLAB P100K'
_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      -0.0398309000
_diffrn_orient_matrix_UB_12      0.0391230000
_diffrn_orient_matrix_UB_13      0.0718806000
_diffrn_orient_matrix_UB_21      -0.0725269000
_diffrn_orient_matrix_UB_22      0.0661406000
_diffrn_orient_matrix_UB_23      -0.0450012000
_diffrn_orient_matrix_UB_31      -0.1043004000
_diffrn_orient_matrix_UB_32      -0.0610227000
_diffrn_orient_matrix_UB_33      -0.0027555000
_diffrn_radiation_monochromator  'Rigaku Osmic Confocal Optical System'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27280
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        66.968
_diffrn_reflns_theta_max         66.968
_diffrn_reflns_theta_min         3.723
_diffrn_source                   'Rotating Anode'
_diffrn_source_type              'Rigaku MM-007HF'
_exptl_absorpt_coefficient_mu    1.586
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72199
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.82a (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    1.131
_exptl_crystal_description       plate
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.032
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         5831
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0487P)^2^+0.7529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.1004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5003
_reflns_number_total             5831
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01298d2.cif
_cod_data_source_block           cbas70
_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               7716116
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.884
_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.a Ternary CH refined with riding coordinates:
 C31(H31), C12(H12), C28(H28), C15(H15)
2.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C18(H18A,H18B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C26(H26), C24(H24), C9(H9), C25(H25), C10(H10), C41(H41),
 C42(H42), C45(H45), C43(H43), C46(H46), C44(H44)
2.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C30(H30A,H30B,H30C), C33(H33A,H33B,H33C), C16(H16A,H16B,
 H16C), C19(H19A,H19B,H19C), C29(H29A,H29B,H29C), C32(H32A,H32B,H32C), C17(H17A,
 H17B,H17C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              4941