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_7718003
_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 N4 O2 Si4 Sr2, C6 H6'
_chemical_formula_sum            'C62 H98 N4 O2 Si4 Sr2'
_chemical_formula_weight         1219.04
_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   geom
_audit_creation_date             2023-12-05
_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                 92.7130(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.63227(12)
_cell_length_b                   10.88063(5)
_cell_length_c                   19.72812(8)
_cell_measurement_reflns_used    52234
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      76.1210
_cell_measurement_theta_min      4.2860
_cell_volume                     6567.98(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (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 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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     -4.00  35.00   1.00    1.00    --  -42.66  19.00 -60.00   39
  2  \w    -22.00   3.00   1.00    1.00    --  -42.66  38.00  30.00   25
  3  \w    -18.00  22.00   1.00    1.00    --  -42.66  38.00  60.00   40
  4  \w    -11.00  27.00   1.00    1.00    --  -42.66  38.00 -30.00   38
  5  \w     -5.00  34.00   1.00    1.00    --  -42.66  19.00 -90.00   39
  6  \w     10.00  35.00   1.00    1.00    --  -42.66  19.00-150.00   25
  7  \w     73.00 106.00   1.00    1.00    --   42.66 178.00   0.00   33
  8  \w     41.00  72.00   1.00    4.00    --  111.00 -45.00 120.00   31
  9  \w     41.00  66.00   1.00    4.00    --  111.00 -45.00 -90.00   25
 10  \w     31.00  87.00   1.00    4.00    --  111.00 -95.00 120.00   56
 11  \w     52.00  78.00   1.00    4.00    --  111.00 -61.00-150.00   26
 12  \w    113.00 154.00   1.00    4.00    --  111.00  77.00 150.00   41
 13  \w     98.00 147.00   1.00    4.00    --  111.00 125.00-180.00   49
 14  \w    100.00 126.00   1.00    4.00    --  111.00  45.00  60.00   26
 15  \w    144.00 177.00   1.00    4.00    --  111.00  30.00-120.00   33
 16  \w    106.00 132.00   1.00    4.00    --  111.00  30.00-120.00   26
 17  \w     54.00 123.00   1.00    4.00    --  111.00 -77.00-150.00   69
 18  \w     47.00  91.00   1.00    4.00    --  111.00 -61.00 -30.00   44
 19  \w     40.00  70.00   1.00    4.00    --  111.00 -45.00-180.00   30
 20  \w     43.00  69.00   1.00    4.00    --  111.00 -61.00-120.00   26
 21  \w     46.00  93.00   1.00    4.00    --  111.00 -61.00 -90.00   47
 22  \w    138.00 171.00   1.00    4.00    --  111.00  77.00 120.00   33
 23  \w    148.00 176.00   1.00    4.00    --  111.00  45.00 -60.00   28
 24  \w     87.00 177.00   1.00    4.00    --  111.00  45.00 -90.00   90
 25  \w     41.00  71.00   1.00    4.00    --  111.00-125.00-120.00   30
 26  \w     97.00 132.00   1.00    4.00    --  111.00  45.00 -60.00   35
 27  \w      0.00  28.00   1.00    1.00    --  -42.66  19.00-180.00   28
 28  \w    -22.00   3.00   1.00    1.00    --  -42.66  38.00-150.00   25
 29  \w     59.00 107.00   1.00    1.00    --   42.66-178.00-120.00   48
 30  \w     66.00 124.00   1.00    1.00    --   42.66 178.00 120.00   58
 31  \w     41.00  79.00   1.00    1.00    --   42.66 -99.00-180.00   38
 32  \w      7.00  34.00   1.00    1.00    --   42.66 -99.00 120.00   27
 33  \w    131.00 168.00   1.00    4.00    --  111.00  15.00-180.00   37
 34  \w     66.00  92.00   1.00    4.00    --  111.00  15.00  30.00   26
 35  \w     39.00  66.00   1.00    4.00    --  111.00-102.00  -9.39   27
 36  \w     78.00 105.00   1.00    4.00    --  111.00 -95.00 150.00   27
 37  \w    105.00 166.00   1.00    4.00    --  111.00  77.00   0.00   61
 38  \w     62.00  87.00   1.00    4.00    --  111.00 -61.00   0.00   25
 39  \w     36.00  65.00   1.00    4.00    --  111.00 -95.00 150.00   29
 40  \w     50.00  76.00   1.00    4.00    --  111.00 -61.00 120.00   26
 41  \w     81.00 107.00   1.00    4.00    --  111.00-101.00 -72.41   26
 42  \w     80.00 112.00   1.00    4.00    --  111.00-125.00-180.00   32
 43  \w     75.00 105.00   1.00    4.00    --  111.00 -95.00  30.00   30
 44  \w     85.00 112.00   1.00    4.00    --  111.00-125.00 120.00   27
 45  \w     40.00  65.00   1.00    4.00    --  111.00 -45.00   0.00   25
 46  \w     32.00  58.00   1.00    4.00    --  111.00 -95.00  30.00   26
 47  \w     69.00 112.00   1.00    4.00    --  111.00-125.00-120.00   43
 48  \w     81.00 106.00   1.00    4.00    --  111.00 -95.00-150.00   25
 49  \w     77.00 112.00   1.00    4.00    --  111.00-125.00  30.00   35
 50  \w     78.00 104.00   1.00    4.00    --  111.00 -95.00   0.00   26
 51  \w     62.00  88.00   1.00    4.00    --  111.00 -61.00  30.00   26
 52  \w     99.00 125.00   1.00    4.00    --  111.00  15.00-180.00   26
 53  \w     42.00  68.00   1.00    4.00    --  111.00-125.00 120.00   26
 54  \w     83.00 108.00   1.00    4.00    --  111.00-102.00  -9.39   25
 55  \w    131.00 167.00   1.00    4.00    --  111.00 125.00 -60.00   36
 56  \w     64.00  90.00   1.00    4.00    --  111.00-125.00   0.00   26
 57  \w     84.00 109.00   1.00    4.00    --  111.00-111.00 -84.83   25
 58  \w    111.00 149.00   1.00    4.00    --  111.00  77.00-180.00   38
 59  \w     41.00  67.00   1.00    4.00    --  111.00-111.00 -84.83   26
 60  \w     61.00  92.00   1.00    1.00    --   42.66 178.00-150.00   31
 61  \w      3.00  30.00   1.00    1.00    --   38.00  88.00-154.53   27
 62  \w   -115.00 -21.00   1.00    1.00    --  -42.66 -38.00-120.00   94
 63  \w    -54.00 -23.00   1.00    1.00    --  -42.66 -38.00  30.00   31
 64  \w    -78.00 -20.00   1.00    1.00    --  -42.66 -38.00 120.00   58
 65  \w   -115.00 -59.00   1.00    1.00    --  -42.66 -38.00  30.00   56
 66  \w     14.00  41.00   1.00    1.00    --   46.00  81.00 120.60   27
 67  \w     15.00  40.00   1.00    1.00    --   46.00  77.00  -7.60   25
 68  \w     14.00  39.00   1.00    1.00    --   46.00  80.00  51.98   25
 69  \w     15.00  42.00   1.00    1.00    --   46.00  79.00 178.22   27
 70  \w     14.00  39.00   1.00    1.00    --   46.00  81.00 -96.86   25
 71  \w     28.00  54.00   1.00    1.00    --   58.00  71.00  26.95   26
 72  \w     28.00  58.00   1.00    1.00    --   58.00  71.00 167.24   30
 73  \w     28.00  54.00   1.00    1.00    --   58.00  70.00 -84.24   26
 74  \w     32.00  58.00   1.00    1.00    --   62.00  71.00  60.32   26
 75  \w     32.00  58.00   1.00    1.00    --   62.00  70.00 122.77   26
 76  \w     36.00  63.00   1.00    1.00    --   66.00  70.00-173.97   27
 77  \w     40.00  66.00   1.00    1.00    --   70.00  70.00 -24.63   26
 78  \w     40.00  66.00   1.00    1.00    --   70.00  70.00-145.37   26
 79  \w     40.00  66.00   1.00    1.00    --   70.00  70.00 -76.73   26
 80  \w     76.00 103.00   1.00    1.00    --   70.00  70.00 -76.73   27
 81  \w     40.00  67.00   1.00    1.00    --   70.00  70.00  69.10   27
 82  \w     44.00  71.00   1.00    1.00    --   70.00  67.00  89.76   27
 83  \w     40.00  66.00   1.00    1.00    --   70.00  70.00 -51.77   26
 84  \w    118.00 144.00   1.00    1.00    --   74.00  64.00 124.01   26
 85  \w     46.00  72.00   1.00    1.00    --   74.00  64.00 124.01   26
 86  \w     45.00  82.00   1.00    1.00    --   74.00  69.00   2.33   37
 87  \w     49.00  75.00   1.00    4.00    --   78.00  66.00-127.31   26
 88  \w     52.00  78.00   1.00    4.00    --   82.00  70.00 121.77   26
 89  \w     53.00 105.00   1.00    4.00    --   82.00  67.00 154.61   52
 90  \w     59.00  84.00   1.00    4.00    --   86.00  63.00 -87.23   25
 91  \w     62.00  88.00   1.00    4.00    --   86.00  47.00  23.28   26
 92  \w     62.00  99.00   1.00    4.00    --   90.00  64.00-162.79   37
 93  \w     64.00  89.00   1.00    4.00    --   90.00  57.00-115.27   25
 94  \w     64.00  97.00   1.00    4.00    --   94.00  70.00 -65.02   33
 95  \w     71.00  97.00   1.00    4.00    --   98.00  58.00  31.16   26
 96  \w     71.00  97.00   1.00    4.00    --   98.00  66.00 103.65   26
 97  \w     74.00 126.00   1.00    4.00    --  102.00  64.00 171.84   52
 98  \w    152.00 177.00   1.00    4.00    --  106.00  68.00  74.86   25
 99  \w     78.00 104.00   1.00    4.00    --  106.00  68.00  74.86   26
100  \w    122.00 178.00   1.00    4.00    --  111.00  61.00  30.00   56
101  \w    137.00 176.00   1.00    4.00    --  111.00  61.00 -60.00   39
102  \w     83.00 109.00   1.00    4.00    --  111.00  61.00 -60.00   26
103  \w     83.00 115.00   1.00    4.00    --  111.00  61.00  30.00   32
104  \w     83.00 169.00   1.00    4.00    --  111.00  61.00  90.00   86
105  \w    139.00 165.00   1.00    4.00    --  111.00  61.00 120.00   26
106  \w    131.00 158.00   1.00    4.00    --  111.00  45.00 -30.00   27
107  \w     91.00 116.00   1.00    4.00    --  111.00  45.00 -30.00   25
108  \w     83.00 111.00   1.00    4.00    --  111.00  61.00-120.00   28
109  \w     83.00 148.00   1.00    4.00    --  111.00  61.00   0.00   65
110  \w     83.00 127.00   1.00    4.00    --  111.00  61.00 120.00   44
111  \w     83.00 111.00   1.00    4.00    --  111.00  61.00-150.00   28
112  \w    143.00 169.00   1.00    4.00    --  111.00  61.00-180.00   26
113  \w     83.00 175.00   1.00    4.00    --  111.00  61.00  60.00   92
114  \w    149.00 175.00   1.00    4.00    --  111.00  61.00 150.00   26
115  \w     83.00 124.00   1.00    4.00    --  111.00  61.00-180.00   41
116  \w     83.00 133.00   1.00    4.00    --  111.00  61.00 150.00   50
117  \w    153.00 178.00   1.00    4.00    --  111.00  61.00 -90.00   25
118  \w     83.00 109.00   1.00    4.00    --  111.00  61.00 -90.00   26
119  \w     83.00 161.00   1.00    4.00    --  111.00  61.00 -30.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0442010000
_diffrn_orient_matrix_UB_12      -0.0069633000
_diffrn_orient_matrix_UB_13      -0.0404888000
_diffrn_orient_matrix_UB_21      0.0139505000
_diffrn_orient_matrix_UB_22      -0.1222973000
_diffrn_orient_matrix_UB_23      -0.0318623000
_diffrn_orient_matrix_UB_31      -0.0196671000
_diffrn_orient_matrix_UB_32      -0.0710227000
_diffrn_orient_matrix_UB_33      0.0587913000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0116
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            84520
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.141
_diffrn_reflns_theta_min         4.313
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.156
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64203
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
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    1.233
_exptl_crystal_description       plate
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.042
_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     346
_refine_ls_number_reflns         6865
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0199
_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^)+(0.0282P)^2^+4.9901P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0523
_refine_ls_wR_factor_ref         0.0541
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6399
_reflns_number_total             6865
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00044k2.cif
_cod_data_source_block           069mhar23
_cod_depositor_comments
'Adding full bibliography for 7718002--7718016.cif.'
_cod_database_code               7718003
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C56 H60 N4 O2 Si4 Sr2'
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.571
_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.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14), C23(H23), C26(H26)
2.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)
2.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              36055
_shelx_hkl_checksum              38976
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.471
_oxdiff_exptl_absorpt_empirical_full_min 0.752