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_7718010
_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 Ca2 N4 O2 Si4, C6 H14'
_chemical_formula_sum            'C62 H106 Ca2 N4 O2 Si4'
_chemical_formula_weight         1132.02
_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             2024-01-22
_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                 92.787(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.405(3)
_cell_length_b                   10.7081(9)
_cell_length_c                   19.7961(13)
_cell_measurement_reflns_used    4917
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      75.2000
_cell_measurement_theta_min      4.4310
_cell_volume                     6649.3(10)
_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 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.980
_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     -5.00  29.00   1.00   10.00    --  -41.15  19.00 -90.00   34
  2  \w    -21.00   5.00   1.00   10.00    --  -41.15  37.00 -60.00   26
  3  \w    -57.00 -19.00   1.00   10.00    --  -41.15 -37.00  30.00   38
  4  \w     -5.00  36.00   1.00   10.00    --  -41.15  19.00 -30.00   41
  5  \w   -114.00 -84.00   1.00   10.00    --  -41.15 -37.00  30.00   30
  6  \w     11.00  36.00   1.00   10.00    --  -41.15  19.00 120.00   25
  7  \w    -39.00  20.00   1.00   10.00    --  -41.15  57.00  30.00   59
  8  \w    108.00 177.00   1.00   40.00    --  111.00  77.00 -30.00   69
  9  \w     40.00  66.00   1.00   40.00    --  111.00 -45.00 -60.00   26
 10  \w     42.00  81.00   1.00   40.00    --  111.00 -61.00 120.00   39
 11  \w     99.00 169.00   1.00   40.00    --  111.00 125.00-120.00   70
 12  \w     31.00  93.00   1.00   40.00    --  111.00 -94.00  30.00   62
 13  \w     42.00  69.00   1.00   40.00    --  111.00 -45.00-150.00   27
 14  \w     98.00 124.00   1.00   40.00    --  111.00 125.00 150.00   26
 15  \w     40.00  71.00   1.00   40.00    --  111.00 -45.00   0.00   31
 16  \w     58.00  92.00   1.00   40.00    --  111.00 -61.00 150.00   34
 17  \w     54.00  86.00   1.00   40.00    --  111.00 -61.00-120.00   32
 18  \w    112.00 155.00   1.00   40.00    --  111.00  77.00-120.00   43
 19  \w    106.00 178.00   1.00   40.00    --  111.00  77.00  60.00   72
 20  \w     42.00  72.00   1.00   40.00    --  111.00 -45.00 -90.00   30
 21  \w     41.00  79.00   1.00   40.00    --  111.00-125.00 -90.00   38
 22  \w     44.00  78.00   1.00   40.00    --  111.00-125.00   0.00   34
 23  \w    126.00 167.00   1.00   40.00    --  111.00  45.00 120.00   41
 24  \w     88.00 113.00   1.00   40.00    --  111.00  45.00 120.00   25
 25  \w      0.00  31.00   1.00   10.00    --  -41.15  19.00-120.00   31
 26  \w    -40.00  23.00   1.00   10.00    --  -41.15  57.00-180.00   63
 27  \w     -5.00  21.00   1.00   10.00    --  -41.15  19.00   0.00   26
 28  \w     42.00  89.00   1.00   10.00    --   41.15-125.00 -30.00   47
 29  \w     53.00  79.00   1.00   10.00    --   41.15-125.00 -60.00   26
 30  \w     33.00  87.00   1.00   10.00    --   41.15-125.00 150.00   54
 31  \w    106.00 175.00   1.00   40.00    --  111.00  77.00   0.00   69
 32  \w     77.00 104.00   1.00   40.00    --  111.00 -94.00 -30.00   27
 33  \w    105.00 153.00   1.00   40.00    --  111.00  77.00-150.00   48
 34  \w     98.00 125.00   1.00   40.00    --  111.00 125.00-180.00   27
 35  \w     77.00 110.00   1.00   40.00    --  111.00-125.00 150.00   33
 36  \w     45.00  77.00   1.00   40.00    --  111.00-125.00  90.00   32
 37  \w     58.00  91.00   1.00   40.00    --  111.00 -61.00 -60.00   33
 38  \w     68.00 107.00   1.00   40.00    --  111.00 -94.00 -90.00   39
 39  \w    138.00 174.00   1.00   40.00    --  111.00  45.00 150.00   36
 40  \w     49.00  96.00   1.00   40.00    --  111.00-125.00-180.00   47
 41  \w     38.00  84.00   1.00   40.00    --  111.00 -77.00-180.00   46
 42  \w     40.00  70.00   1.00   40.00    --  111.00 -45.00  30.00   30
 43  \w     77.00 112.00   1.00   40.00    --  111.00-125.00   0.00   35
 44  \w     41.00  66.00   1.00   40.00    --  111.00 -61.00 -30.00   25
 45  \w     67.00 106.00   1.00   40.00    --  111.00 -94.00-180.00   39
 46  \w    148.00 176.00   1.00   40.00    --  111.00 125.00-180.00   28
 47  \w    100.00 173.00   1.00   40.00    --  111.00  45.00 -60.00   73
 48  \w     82.00 107.00   1.00   40.00    --  111.00 -94.00 120.00   25
 49  \w     81.00 107.00   1.00   40.00    --  111.00 -94.00  30.00   26
 50  \w     41.00  67.00   1.00   40.00    --  111.00-125.00-150.00   26
 51  \w     75.00 112.00   1.00   40.00    --  111.00-125.00 -90.00   37
 52  \w     73.00 107.00   1.00   40.00    --  111.00 -94.00-120.00   34
 53  \w     32.00  64.00   1.00   40.00    --  111.00 -94.00 120.00   32
 54  \w    151.00 178.00   1.00   40.00    --  111.00  45.00 120.00   27
 55  \w      2.00  27.00   1.00   10.00    --   38.00  90.00 133.48   25
 56  \w    -17.00  31.00   1.00   10.00    --  -41.15  37.00  90.00   48
;
_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      -0.0464713000
_diffrn_orient_matrix_UB_12      -0.0275497000
_diffrn_orient_matrix_UB_13      0.0167726000
_diffrn_orient_matrix_UB_21      0.0037883000
_diffrn_orient_matrix_UB_22      0.0939717000
_diffrn_orient_matrix_UB_23      0.0590418000
_diffrn_orient_matrix_UB_31      -0.0153945000
_diffrn_orient_matrix_UB_32      0.1055534000
_diffrn_orient_matrix_UB_33      -0.0479390000
_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  0.1048
_diffrn_reflns_av_unetI/netI     0.0661
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            40355
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.495
_diffrn_reflns_theta_min         4.363
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.492
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69547
_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    1.131
_exptl_crystal_description       Shard
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         6929
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_gt           0.0584
_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^)+(0.0912P)^2^+3.8214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1487
_refine_ls_wR_factor_ref         0.1835
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4365
_reflns_number_total             6929
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00044k2.cif
_cod_data_source_block           002mdh24
_cod_depositor_comments
'Adding full bibliography for 7718002--7718016.cif.'
_cod_database_code               7718010
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C52 H92 Ca2 N4 O2 Si4'
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.700
_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:
 C11(H11), C14(H14), C23(H23), C26(H26)
2.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C31(H31A,H31B)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C19(H19), C20(H20), C21(H21)
2.d 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), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              20693
_shelx_hkl_checksum              27398
_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 1.641
_oxdiff_exptl_absorpt_empirical_full_min 0.697