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_7718013
_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, 1[C6H14]'
_chemical_formula_sum            'C62 H106 N4 O2 Si4 Sr2'
_chemical_formula_weight         1227.10
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-06
_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                 93.4400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.1544(2)
_cell_length_b                   10.98160(10)
_cell_length_c                   19.78100(10)
_cell_measurement_reflns_used    40461
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      76.0210
_cell_measurement_theta_min      4.2330
_cell_volume                     6755.38(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.95a (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 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_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 0.994
_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   -114.00 -20.00   1.00    1.00    --  -42.41 -38.00 -60.00   94
  2  \w    -21.00  27.00   1.00    1.00    --  -42.41  38.00  90.00   48
  3  \w     -1.00  26.00   1.00    1.00    --  -42.41  19.00 -60.00   27
  4  \w     -4.00  27.00   1.00    1.00    --  -42.41  19.00  60.00   31
  5  \w     63.00 101.00   1.00    1.00    --   42.41-133.00 -46.00   38
  6  \w     44.00  71.00   1.00    4.00    --  111.00 -45.00-150.00   27
  7  \w     40.00  65.00   1.00    4.00    --  111.00 -45.00 -90.00   25
  8  \w     41.00  72.00   1.00    4.00    --  111.00 -45.00 -60.00   31
  9  \w     87.00 176.00   1.00    4.00    --  111.00  30.00 -30.00   89
 10  \w     44.00  71.00   1.00    4.00    --  111.00 -45.00-180.00   27
 11  \w    103.00 152.00   1.00    4.00    --  111.00  30.00-120.00   49
 12  \w     50.00 106.00   1.00    4.00    --  111.00 -95.00  30.00   56
 13  \w     40.00  72.00   1.00    4.00    --  111.00 -45.00  30.00   32
 14  \w     72.00 112.00   1.00    4.00    --  111.00-125.00 150.00   40
 15  \w    107.00 176.00   1.00    4.00    --  111.00  45.00-180.00   69
 16  \w     41.00  72.00   1.00    4.00    --  111.00 -45.00 150.00   31
 17  \w     57.00  98.00   1.00    4.00    --  111.00-125.00 -30.00   41
 18  \w     43.00  94.00   1.00    4.00    --  111.00-125.00-180.00   51
 19  \w    123.00 168.00   1.00    4.00    --  111.00  77.00  60.00   45
 20  \w     60.00  93.00   1.00    4.00    --  111.00 -61.00   0.00   33
 21  \w      4.00  34.00   1.00    1.00    --  -42.41  19.00  30.00   30
 22  \w      3.00  30.00   1.00    1.00    --  -42.41  19.00-180.00   27
 23  \w    -84.00 -20.00   1.00    1.00    --  -42.41 -38.00-150.00   64
 24  \w    -21.00   4.00   1.00    1.00    --  -42.41  38.00 150.00   25
 25  \w     16.00  59.00   1.00    1.00    --   42.41 -99.00  90.00   43
 26  \w     61.00 115.00   1.00    1.00    --   42.41 178.00 -90.00   54
 27  \w     73.00 100.00   1.00    4.00    --  111.00  15.00  60.00   27
 28  \w     88.00 132.00   1.00    4.00    --  111.00  30.00 120.00   44
 29  \w     31.00  56.00   1.00    4.00    --  111.00 -95.00-180.00   25
 30  \w     72.00 109.00   1.00    4.00    --  111.00-125.00 -60.00   37
 31  \w     58.00  91.00   1.00    4.00    --  111.00 -61.00 120.00   33
 32  \w    142.00 167.00   1.00    4.00    --  111.00 125.00 -30.00   25
 33  \w     87.00 112.00   1.00    4.00    --  111.00-125.00 -30.00   25
 34  \w    132.00 166.00   1.00    4.00    --  111.00  15.00  60.00   34
 35  \w     40.00  65.00   1.00    4.00    --  111.00 -45.00-120.00   25
 36  \w     43.00  70.00   1.00    4.00    --  111.00-125.00 -60.00   27
 37  \w     81.00 106.00   1.00    4.00    --  111.00 -95.00 120.00   25
 38  \w     40.00  67.00   1.00    4.00    --  111.00 -95.00 120.00   27
 39  \w     98.00 157.00   1.00    4.00    --  111.00 125.00  90.00   59
 40  \w    109.00 136.00   1.00    4.00    --  111.00  77.00-180.00   27
 41  \w    142.00 171.00   1.00    4.00    --  111.00  77.00-180.00   29
 42  \w    127.00 172.00   1.00    4.00    --  111.00  77.00 -90.00   45
 43  \w     74.00 118.00   1.00    4.00    --  111.00 -77.00-120.00   44
 44  \w     77.00 104.00   1.00    4.00    --  111.00-125.00 -90.00   27
 45  \w     74.00 112.00   1.00    4.00    --  111.00-125.00  30.00   38
 46  \w     80.00 122.00   1.00    4.00    --  111.00-137.00 136.00   42
 47  \w     74.00 106.00   1.00    4.00    --  111.00 -95.00-180.00   32
 48  \w     86.00 112.00   1.00    4.00    --  111.00-125.00  60.00   26
 49  \w     42.00  67.00   1.00    4.00    --  111.00-125.00  60.00   25
 50  \w      6.00  31.00   1.00    1.00    --   38.00  79.00 -91.49   25
 51  \w      3.00  29.00   1.00    1.00    --   38.00  87.00 -45.06   26
 52  \w    -19.00  30.00   1.00    1.00    --  -42.41  38.00-120.00   49
 53  \w   -114.00 -27.00   1.00    1.00    --  -42.41 -38.00 120.00   87
 54  \w     60.00 128.00   1.00    1.00    --   42.41-178.00  60.00   68
 55  \w     13.00  38.00   1.00    1.00    --   46.00  82.00-133.11   25
 56  \w     15.00  40.00   1.00    1.00    --   46.00  77.00  90.77   25
 57  \w     14.00  39.00   1.00    1.00    --   46.00  81.00 137.44   25
 58  \w     21.00  51.00   1.00    1.00    --   50.00  66.00  54.96   30
 59  \w     29.00  59.00   1.00    1.00    --   58.00  68.00-179.26   30
 60  \w    102.00 130.00   1.00    1.00    --   62.00  70.00 -22.18   28
 61  \w     33.00  67.00   1.00    1.00    --   62.00  70.00 -22.18   34
 62  \w     34.00  68.00   1.00    1.00    --   62.00  67.00  28.57   34
 63  \w     36.00  63.00   1.00    1.00    --   66.00  70.00-107.63   27
 64  \w     36.00  64.00   1.00    1.00    --   66.00  70.00-145.73   28
 65  \w     39.00  86.00   1.00    1.00    --   66.00  71.00 125.67   47
 66  \w    113.00 138.00   1.00    1.00    --   66.00  71.00 125.67   25
 67  \w     36.00  70.00   1.00    1.00    --   66.00  71.00 -54.43   34
 68  \w     40.00 119.00   1.00    1.00    --   70.00  71.00  62.81   79
 69  \w     41.00  86.00   1.00    1.00    --   70.00  70.00 100.30   45
 70  \w     42.00  77.00   1.00    1.00    --   70.00  70.00 -83.82   35
 71  \w     45.00  82.00   1.00    1.00    --   74.00  69.00 -96.89   37
 72  \w     83.00 110.00   1.00    4.00    --  111.00  61.00 -60.00   27
 73  \w     83.00 109.00   1.00    4.00    --  111.00  61.00  30.00   26
 74  \w    126.00 155.00   1.00    4.00    --  111.00  45.00 -90.00   29
 75  \w     83.00 109.00   1.00    4.00    --  111.00  61.00-180.00   26
 76  \w     83.00 110.00   1.00    4.00    --  111.00  61.00 -90.00   27
 77  \w    126.00 161.00   1.00    4.00    --  111.00  61.00  30.00   35
 78  \w     88.00 117.00   1.00    4.00    --  111.00  45.00 -90.00   29
 79  \w    134.00 178.00   1.00    4.00    --  111.00  61.00 -60.00   44
 80  \w    119.00 170.00   1.00    4.00    --  111.00  61.00   0.00   51
 81  \w     89.00 116.00   1.00    4.00    --  111.00  45.00 -60.00   27
 82  \w    140.00 167.00   1.00    4.00    --  111.00  45.00-150.00   27
 83  \w     83.00 112.00   1.00    4.00    --  111.00  61.00   0.00   29
 84  \w    140.00 171.00   1.00    4.00    --  111.00  45.00 150.00   31
 85  \w    126.00 177.00   1.00    4.00    --  111.00  61.00-120.00   51
 86  \w     83.00 109.00   1.00    4.00    --  111.00  61.00-120.00   26
 87  \w     87.00 123.00   1.00    4.00    --  111.00  45.00 150.00   36
 88  \w     91.00 118.00   1.00    4.00    --  111.00  45.00-180.00   27
 89  \w     88.00 115.00   1.00    4.00    --  111.00  45.00 -30.00   27
 90  \w     83.00 109.00   1.00    4.00    --  111.00  61.00 150.00   26
 91  \w     84.00 119.00   1.00    4.00    --  111.00  61.00-150.00   35
 92  \w     89.00 116.00   1.00    4.00    --  111.00  45.00   0.00   27
 93  \w    132.00 159.00   1.00    4.00    --  111.00  45.00   0.00   27
 94  \w     87.00 120.00   1.00    4.00    --  111.00  45.00  60.00   33
 95  \w     89.00 116.00   1.00    4.00    --  111.00  45.00-150.00   27
 96  \w    153.00 178.00   1.00    4.00    --  111.00  61.00 120.00   25
 97  \w     83.00 122.00   1.00    4.00    --  111.00  61.00  60.00   39
 98  \w     83.00 130.00   1.00    4.00    --  111.00  61.00 120.00   47
 99  \w    134.00 165.00   1.00    4.00    --  111.00  61.00  90.00   31
100  \w    153.00 178.00   1.00    4.00    --  111.00  61.00 -30.00   25
101  \w     83.00 113.00   1.00    4.00    --  111.00  61.00  90.00   30
102  \w     83.00 109.00   1.00    4.00    --  111.00  61.00 -30.00   26
;
_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      -0.0485264000
_diffrn_orient_matrix_UB_12      -0.0064042000
_diffrn_orient_matrix_UB_13      -0.0198742000
_diffrn_orient_matrix_UB_21      0.0099792000
_diffrn_orient_matrix_UB_22      -0.0217041000
_diffrn_orient_matrix_UB_23      -0.0743840000
_diffrn_orient_matrix_UB_31      0.0006818000
_diffrn_orient_matrix_UB_32      -0.1384355000
_diffrn_orient_matrix_UB_33      0.0125869000
_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  0.0347
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            76112
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.345
_diffrn_reflns_theta_min         4.270
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.069
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.95a (Rigaku Oxford Diffraction, 2023)
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    1.207
_exptl_crystal_description       block
_exptl_crystal_F_000             2616
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         7046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0383P)^2^+8.0342P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0787
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6211
_reflns_number_total             7046
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00044k2.cif
_cod_data_source_block           005mdh24
_cod_depositor_comments
'Adding full bibliography for 7718002--7718016.cif.'
_cod_database_code               7718013
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C52 H92 Sr2 N4 O2 Si4'
_shelx_estimated_absorpt_t_max   0.862
_shelx_estimated_absorpt_t_min   0.658
_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)
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)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 188 electrons were 
found in a volume of 1084\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
0.5[C6H14] per Asymmetric Unit 
which account for 200 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              16601
_shelx_hkl_checksum              5155
_shelx_fab_checksum              85154
_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 1.337
_oxdiff_exptl_absorpt_empirical_full_min 0.789