Heavier alkaline earth and heterobimetallic s-block "ate" complexes of a di(amido)siloxane ligand: solid-state structure and dynamic solution-phase behaviour.
Haynes, Matthew D.; O'Reilly, Andrea; Poole, Alice J. M.; Roper, Aisling F.; Thum, Stefan; Morris, Louis J.; Coles, Martyn P.; Fulton, J. Robin; Harder, Sjoerd; Turner, Zoë R; O'Hare, Dermot; Dalton transactions (Cambridge, England : 2003) 54 (2025) 4542–4555; doi:10.1039/d5dt00044k

data_7718005
_publ_section_title
;
 Heavier alkaline earth and heterobimetallic s-block "ate" complexes of a
 di(amido)siloxane ligand: solid-state structure and dynamic
 solution-phase behaviour.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4542
_journal_page_last               4555
_journal_paper_doi               10.1039/d5dt00044k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C56 H92 Ba2 N4 O2 Si4, C6 H6'
_chemical_formula_sum            'C62 H98 Ba2 N4 O2 Si4'
_chemical_formula_weight         1318.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-12-06
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-12-18 deposited with the CCDC.	2025-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.5715(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.62654(9)
_cell_length_b                   11.41698(4)
_cell_length_c                   20.02024(7)
_cell_measurement_reflns_used    63460
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      76.1470
_cell_measurement_theta_min      4.1150
_cell_volume                     6758.61(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 10.4102
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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    -44.00   5.00   1.00    1.00    --  -42.66  57.00  90.00   49
  2  \w   -121.00  -8.00   1.00    1.00    --  -42.66 -19.00 120.00  113
  3  \w     97.00 122.00   1.00    1.00    --   42.66 178.00 150.00   25
  4  \w     68.00 127.00   1.00    1.00    --   42.66 178.00  30.00   59
  5  \w     41.00  70.00   1.00    4.00    --  111.00 -45.00  60.00   29
  6  \w     55.00 110.00   1.00    4.00    --  111.00-125.00  90.00   55
  7  \w    110.00 177.00   1.00    4.00    --  111.00  77.00  60.00   67
  8  \w     42.00  72.00   1.00    4.00    --  111.00 -45.00 -30.00   30
  9  \w     40.00  65.00   1.00    4.00    --  111.00 -45.00  30.00   25
 10  \w    106.00 174.00   1.00    4.00    --  111.00  77.00 -90.00   68
 11  \w     93.00 157.00   1.00    4.00    --  111.00  30.00  60.00   64
 12  \w     51.00 109.00   1.00    4.00    --  111.00-125.00  30.00   58
 13  \w     99.00 177.00   1.00    4.00    --  111.00  30.00-180.00   78
 14  \w     83.00 124.00   1.00    4.00    --  111.00 -77.00 -30.00   41
 15  \w     47.00  72.00   1.00    4.00    --  111.00 -45.00 150.00   25
 16  \w     42.00  88.00   1.00    4.00    --  111.00-125.00   0.00   46
 17  \w     31.00  73.00   1.00    4.00    --  111.00 -95.00 -90.00   42
 18  \w    134.00 178.00   1.00    4.00    --  111.00 125.00-120.00   44
 19  \w     56.00  81.00   1.00    4.00    --  111.00 -61.00 -30.00   25
 20  \w     -2.00  36.00   1.00    1.00    --  -42.66  19.00 -60.00   38
 21  \w     -4.00  30.00   1.00    1.00    --  -42.66  19.00 -90.00   34
 22  \w   -108.00 -58.00   1.00    1.00    --  -42.66-178.00 -90.00   50
 23  \w     62.00  87.00   1.00    1.00    --   42.66 178.00   0.00   25
 24  \w     81.00 122.00   1.00    1.00    --   42.66 178.00-120.00   41
 25  \w     43.00  69.00   1.00    4.00    --  111.00-125.00-120.00   26
 26  \w     97.00 128.00   1.00    4.00    --  111.00 125.00-150.00   31
 27  \w     61.00 108.00   1.00    4.00    --  111.00-108.00 -43.12   47
 28  \w     82.00 108.00   1.00    4.00    --  111.00-107.00  28.54   26
 29  \w     44.00  70.00   1.00    4.00    --  111.00 -45.00-180.00   26
 30  \w    148.00 174.00   1.00    4.00    --  111.00 125.00-150.00   26
 31  \w     49.00  87.00   1.00    4.00    --  111.00 -61.00 120.00   38
 32  \w    140.00 166.00   1.00    4.00    --  111.00  77.00 150.00   26
 33  \w     71.00 112.00   1.00    4.00    --  111.00-125.00-120.00   41
 34  \w    102.00 128.00   1.00    4.00    --  111.00-149.00 143.10   26
 35  \w     87.00 112.00   1.00    4.00    --  111.00-125.00 150.00   25
 36  \w     43.00  69.00   1.00    4.00    --  111.00-125.00 150.00   26
 37  \w     42.00  68.00   1.00    4.00    --  111.00 -45.00 120.00   26
 38  \w    115.00 141.00   1.00    4.00    --  111.00 125.00  90.00   26
 39  \w    146.00 172.00   1.00    4.00    --  111.00 125.00  90.00   26
 40  \w     73.00 107.00   1.00    4.00    --  111.00-111.00 -65.91   34
 41  \w     43.00  69.00   1.00    4.00    --  111.00-111.00 -65.91   26
 42  \w    104.00 170.00   1.00    4.00    --  111.00  77.00 120.00   66
 43  \w     60.00 107.00   1.00    4.00    --  111.00-101.00-126.01   47
 44  \w    106.00 133.00   1.00    4.00    --  111.00 125.00   0.00   27
 45  \w    151.00 177.00   1.00    4.00    --  111.00 125.00   0.00   26
 46  \w     70.00 108.00   1.00    4.00    --  111.00-105.00 157.74   38
 47  \w    134.00 173.00   1.00    4.00    --  111.00  45.00  90.00   39
 48  \w     40.00  65.00   1.00    4.00    --  111.00 -45.00 150.00   25
 49  \w     86.00 112.00   1.00    4.00    --  111.00-125.00  30.00   26
 50  \w     83.00 108.00   1.00    4.00    --  111.00-104.00  75.36   25
 51  \w      1.00  27.00   1.00    1.00    --   34.00  85.00  26.99   26
 52  \w    -78.00 -23.00   1.00    1.00    --  -42.66 -38.00 -90.00   55
 53  \w   -114.00 -82.00   1.00    1.00    --  -42.66 -38.00 -90.00   32
 54  \w    -42.00 -16.00   1.00    1.00    --  -42.66 -57.00-180.00   26
 55  \w     84.00 114.00   1.00    1.00    --   42.66  38.00   0.00   30
 56  \w     20.00  73.00   1.00    1.00    --   42.66  38.00   0.00   53
 57  \w     14.00  39.00   1.00    1.00    --   46.00  80.00-150.44   25
 58  \w     13.00  38.00   1.00    1.00    --   46.00  82.00 -94.17   25
 59  \w     13.00  38.00   1.00    1.00    --   46.00  82.00  79.80   25
 60  \w     14.00  39.00   1.00    1.00    --   46.00  80.00 156.51   25
 61  \w     15.00  42.00   1.00    1.00    --   46.00  82.00 -26.38   27
 62  \w     28.00  54.00   1.00    1.00    --   58.00  70.00 128.32   26
 63  \w     61.00  87.00   1.00    1.00    --   58.00  70.00 -76.27   26
 64  \w    105.00 130.00   1.00    1.00    --   58.00  70.00 -76.27   25
 65  \w     29.00  54.00   1.00    1.00    --   58.00  70.00 -76.27   25
 66  \w     32.00  58.00   1.00    1.00    --   62.00  71.00-163.53   26
 67  \w     33.00  59.00   1.00    1.00    --   62.00  69.00  29.35   26
 68  \w     37.00  64.00   1.00    1.00    --   66.00  69.00  66.56   27
 69  \w     36.00  62.00   1.00    1.00    --   66.00  71.00-124.79   26
 70  \w     36.00  62.00   1.00    1.00    --   66.00  71.00 -36.43   26
 71  \w     40.00  66.00   1.00    1.00    --   70.00  71.00 158.44   26
 72  \w     40.00  66.00   1.00    1.00    --   70.00  71.00  76.72   26
 73  \w     40.00  66.00   1.00    1.00    --   70.00  71.00 -58.02   26
 74  \w     41.00  68.00   1.00    1.00    --   70.00  68.00 129.30   27
 75  \w    116.00 142.00   1.00    1.00    --   70.00  71.00 -58.02   26
 76  \w     40.00  66.00   1.00    1.00    --   70.00  70.00 -89.26   26
 77  \w     45.00  71.00   1.00    1.00    --   74.00  68.00  38.10   26
 78  \w    109.00 149.00   1.00    4.00    --   78.00  70.00 -22.29   40
 79  \w     48.00  80.00   1.00    4.00    --   78.00  70.00 -22.29   32
 80  \w     48.00  76.00   1.00    4.00    --   78.00  70.00 102.14   28
 81  \w     52.00  79.00   1.00    4.00    --   82.00  70.00-164.93   27
 82  \w     54.00  81.00   1.00    4.00    --   82.00  62.00-176.38   27
 83  \w     54.00  80.00   1.00    4.00    --   82.00  62.00 158.71   26
 84  \w     59.00  84.00   1.00    4.00    --   86.00  64.00 -61.87   25
 85  \w    121.00 147.00   1.00    4.00    --   86.00  64.00 -61.87   26
 86  \w     58.00  94.00   1.00    4.00    --   86.00  69.00  38.55   36
 87  \w     62.00 121.00   1.00    4.00    --   90.00  65.00-109.08   59
 88  \w     64.00  90.00   1.00    4.00    --   90.00  52.00  93.56   26
 89  \w     66.00  92.00   1.00    4.00    --   94.00  62.00-139.35   26
 90  \w     68.00  94.00   1.00    4.00    --   94.00  54.00 172.17   26
 91  \w     66.00  93.00   1.00    4.00    --   94.00  68.00 -96.79   27
 92  \w     66.00  92.00   1.00    4.00    --   94.00  63.00 124.96   26
 93  \w     73.00 100.00   1.00    4.00    --   98.00  53.00 -35.93   27
 94  \w    131.00 157.00   1.00    4.00    --  102.00  67.00  15.04   26
 95  \w     73.00  99.00   1.00    4.00    --  102.00  67.00  15.04   26
 96  \w     77.00 112.00   1.00    4.00    --  106.00  68.00-105.00   35
 97  \w     84.00 110.00   1.00    4.00    --  111.00  60.00  83.33   26
 98  \w    149.00 175.00   1.00    4.00    --  111.00  61.00-180.00   26
 99  \w     83.00 130.00   1.00    4.00    --  111.00  61.00-180.00   47
100  \w    153.00 178.00   1.00    4.00    --  111.00  61.00 -90.00   25
101  \w     83.00 141.00   1.00    4.00    --  111.00  61.00 -90.00   58
102  \w     83.00 176.00   1.00    4.00    --  111.00  61.00-150.00   93
103  \w     83.00 111.00   1.00    4.00    --  111.00  61.00 150.00   28
104  \w    153.00 178.00   1.00    4.00    --  111.00  61.00  30.00   25
105  \w     83.00 112.00   1.00    4.00    --  111.00  61.00  30.00   29
106  \w    115.00 167.00   1.00    4.00    --  111.00  61.00 -30.00   52
107  \w     84.00 133.00   1.00    4.00    --  111.00  61.00  90.00   49
108  \w     83.00 148.00   1.00    4.00    --  111.00  61.00   0.00   65
109  \w     83.00 109.00   1.00    4.00    --  111.00  61.00 -30.00   26
110  \w    153.00 178.00   1.00    4.00    --  111.00  61.00  60.00   25
111  \w    112.00 137.00   1.00    4.00    --  111.00  64.00 -20.38   25
112  \w     83.00 116.00   1.00    4.00    --  111.00  61.00  60.00   33
113  \w     83.00 110.00   1.00    4.00    --  111.00  64.00 -20.38   27
114  \w    149.00 175.00   1.00    4.00    --  111.00  61.00-120.00   26
115  \w     84.00 137.00   1.00    4.00    --  111.00  61.00-120.00   53
116  \w     83.00 137.00   1.00    4.00    --  111.00  61.00 120.00   54
117  \w     83.00 178.00   1.00    4.00    --  111.00  61.00 -60.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            89686
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.187
_diffrn_reflns_theta_min         4.151
_exptl_absorpt_coefficient_mu    9.991
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.497
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       block
_exptl_crystal_F_000             2728
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         7053
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0175
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+5.3095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0455
_refine_ls_wR_factor_ref         0.0457
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6907
_reflns_number_total             7053
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00044k2.cif
_cod_data_source_block           051mhar23
_cod_depositor_comments
'Adding full bibliography for 7718002--7718016.cif.'
_cod_database_code               7718005
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.316
_shelx_estimated_absorpt_t_min   0.173
_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. Uiso/Uaniso restraints and constraints
Si1 \\sim C1 \\sim C2: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01 within 2A
C10 \\sim C14 \\sim C15 \\sim C16: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 2A
3.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14), C26(H26)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C19(H19), C20(H20), C21(H21), C29(H29), C30(H30),
 C31(H31)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C12(H12A,
 H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C)
;
_shelx_res_checksum              72065
_shelx_hkl_checksum              75581
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;