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_7716108
_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 Br N2 Si'
_chemical_formula_sum            'C31 H45 Br N2 Si'
_chemical_formula_weight         553.69
_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             2023-11-30
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-04-30 deposited with the CCDC.	2024-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.1595(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.96708(12)
_cell_length_b                   22.4804(2)
_cell_length_c                   13.98249(18)
_cell_measurement_reflns_used    37406
_cell_measurement_temperature    173
_cell_measurement_theta_max      66.2810
_cell_measurement_theta_min      1.9680
_cell_volume                     2993.51(6)
_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 2019/3 (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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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    -20.00  35.00   1.00    1.00    --    0.00  77.00 -30.00   55
  2  \w    -20.00  35.00   1.00    1.00    --    0.00  77.00  30.00   55
  3  \w    -12.00  89.00   1.00    1.00    --    0.00  57.00 120.00  101
  4  \w    -15.00  35.00   1.00    1.00    --    5.00  77.00 -90.00   50
  5  \w    -78.00   9.00   1.00    1.00    --    5.00 -37.00 -30.00   87
  6  \w   -141.00 -25.00   1.00    1.00    --  -57.40 -57.00 -60.00  116
  7  \w   -141.00 -88.00   1.00    1.00    --  -57.40 -77.00-120.00   53
  8  \w   -141.00 -88.00   1.00    1.00    --  -57.40 -77.00   0.00   53
  9  \w    -70.00  32.00   1.00    1.00    --  -57.40  57.00  60.00  102
 10  \w    -78.00  32.00   1.00    1.00    --  -57.40  77.00-150.00  110
 11  \w    -72.00   6.00   1.00    1.00    --  -83.30  19.00-150.00   78
 12  \w   -101.00   6.00   1.00    1.00    --  -83.30  77.00  90.00  107
 13  \w   -101.00   6.00   1.00    1.00    --  -83.30  77.00 -60.00  107
 14  \w   -101.00   6.00   1.00    1.00    --  -83.30  77.00 -60.00  107
 15  \w    -97.00 -20.00   1.00    1.00    -- -109.20  82.00  -7.16   77
 16  \w    -98.00 -20.00   1.00    1.00    -- -109.20  79.00-103.76   78
 17  \w   -193.00 -96.00   1.00    1.00    -- -109.20 -45.00 -65.08   97
 18  \w   -193.00 -73.00   1.00    1.00    -- -109.20 -67.00-166.00  120
 19  \w    -94.00 -20.00   1.00    1.00    -- -109.20  13.00 -61.51   74
 20  \w    -97.00 -20.00   1.00    1.00    -- -109.20   6.00 -75.08   77
 21  \w   -193.00 -77.00   1.00    1.00    -- -109.20 -57.00  20.52  116
 22  \w   -193.00-105.00   1.00    1.00    -- -109.20 -37.00 -30.00   88
 23  \w   -122.00 -20.00   1.00    1.00    -- -109.20  58.00  17.73  102
 24  \w    -97.00 -20.00   1.00    1.00    -- -109.20  82.00  63.79   77
 25  \w    -97.00 -20.00   1.00    1.00    -- -109.20  82.00 176.77   77
 26  \w   -100.00 -20.00   1.00    1.00    -- -109.20  21.00-137.67   80
 27  \w   -193.00 -94.00   1.00    1.00    -- -109.20 -46.00 -38.66   99
 28  \w   -125.00 -20.00   1.00    1.00    -- -109.20  64.00 -64.00  105
 29  \w    -98.00 -20.00   1.00    1.00    -- -109.20  81.00 -32.84   78
 30  \w    -97.00 -20.00   1.00    1.00    -- -109.20  82.00 161.46   77
 31  \w   -101.00 -20.00   1.00    1.00    -- -109.20  77.00  30.00   81
 32  \w    -97.00 -20.00   1.00    1.00    -- -109.20  82.00  44.52   77
 33  \w   -193.00-105.00   1.00    1.00    -- -109.20 -37.00 -90.00   88
 34  \w    -98.00 -20.00   1.00    1.00    -- -109.20  80.00 -59.69   78
 35  \w   -101.00 -20.00   1.00    1.00    -- -109.20  77.00-120.00   81
 36  \w   -122.00 -20.00   1.00    1.00    -- -109.20  57.00 -30.00  102
 37  \w   -101.00 -20.00   1.00    1.00    -- -109.20  77.00 120.00   81
 38  \w   -142.00 -80.00   1.00    1.00    -- -109.20 -60.00 -12.97   62
 39  \w   -192.00-161.00   1.00    1.00    -- -109.20 -19.00-120.00   31
 40  \w   -112.00 -86.00   1.00    1.00    -- -109.20  66.00  76.69   26
 41  \w   -146.00 -92.00   1.00    1.00    -- -109.20 -49.00  -7.81   54
 42  \w   -193.00-160.00   1.00    1.00    -- -109.20 -60.00 -12.97   33
 43  \w    -77.00 -52.00   1.00    1.00    -- -109.20   5.00  79.83   25
 44  \w   -193.00-132.00   1.00    1.00    -- -109.20 -63.00 107.59   61
 45  \w   -170.00-144.00   1.00    1.00    -- -109.20 -59.00   0.80   26
 46  \w   -103.00 -78.00   1.00    1.00    -- -109.20 -59.00   0.80   25
 47  \w    -91.00 -40.00   1.00    1.00    -- -109.20  82.00  86.83   51
 48  \w    -87.00 -55.00   1.00    1.00    -- -109.20  61.00-169.75   32
 49  \w    -96.00 -53.00   1.00    1.00    -- -109.20  82.00-165.65   43
;
_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      -0.1093396000
_diffrn_orient_matrix_UB_12      0.0384387000
_diffrn_orient_matrix_UB_13      0.0296577000
_diffrn_orient_matrix_UB_21      -0.0760123000
_diffrn_orient_matrix_UB_22      -0.0567081000
_diffrn_orient_matrix_UB_23      0.0177569000
_diffrn_orient_matrix_UB_31      0.0918285000
_diffrn_orient_matrix_UB_32      -0.0012574000
_diffrn_orient_matrix_UB_33      0.1100467000
_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  0.0182
_diffrn_reflns_av_unetI/netI     0.0087
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            52040
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        66.776
_diffrn_reflns_theta_max         66.776
_diffrn_reflns_theta_min         3.849
_diffrn_source                   'Rotating Anode'
_diffrn_source_type              'Rigaku MM-007HF'
_exptl_absorpt_coefficient_mu    2.396
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75363
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       prism
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         5256
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0349P)^2^+1.5820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0758
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5171
_reflns_number_total             5256
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01298d2.cif
_cod_data_source_block           cbas69
_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               7716108
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.646
_shelx_estimated_absorpt_t_min   0.327
_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. Others
 Sof(Br1A)=1-FVAR(1)
 Sof(Br1)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C28(H28), C31(H31)
3.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C20(H20A,H20B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C24(H24), C25(H25), C26(H26)
3.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              31285