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_7718008
_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         'C34 H64 K N3 O Si4 Sr'
_chemical_formula_sum            'C34 H64 K N3 O Si4 Sr'
_chemical_formula_weight         769.96
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-27
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.5555(2)
_cell_length_b                   20.6930(2)
_cell_length_c                   16.8114(2)
_cell_measurement_reflns_used    39587
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      76.3940
_cell_measurement_theta_min      3.7690
_cell_volume                     8542.33(15)
_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 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 0.996
_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     -1.00  36.00   1.00    3.00    --  -41.52  19.00-120.00   37
  2  \w     -3.00  31.00   1.00    3.00    --  -41.52  19.00  30.00   34
  3  \w      2.00  31.00   1.00    3.00    --  -41.52  19.00 -90.00   29
  4  \w     -2.00  24.00   1.00    3.00    --  -41.52  19.00 -60.00   26
  5  \w     -5.00  22.00   1.00    3.00    --  -41.52  19.00 150.00   27
  6  \w    -19.00  18.00   1.00    3.00    --  -41.52  37.00-180.00   37
  7  \w     58.00  84.00   1.00   14.00    --  111.00 -61.00  60.00   26
  8  \w     51.00  77.00   1.00   14.00    --  111.00 -59.00-106.00   26
  9  \w     42.00 117.00   1.00   14.00    --  111.00 -77.00 150.00   75
 10  \w     40.00  65.00   1.00   14.00    --  111.00 -45.00  60.00   25
 11  \w     40.00  65.00   1.00   14.00    --  111.00 -45.00   0.00   25
 12  \w    106.00 174.00   1.00   14.00    --  111.00  77.00 150.00   68
 13  \w     41.00  68.00   1.00   14.00    --  111.00 -45.00 -90.00   27
 14  \w     46.00  90.00   1.00   14.00    --  111.00 -61.00  30.00   44
 15  \w    103.00 172.00   1.00   14.00    --  111.00  77.00  60.00   69
 16  \w     32.00  90.00   1.00    3.00    --   41.52-125.00  30.00   58
 17  \w     27.00  76.00   1.00    3.00    --   41.52 -99.00-180.00   49
 18  \w    107.00 170.00   1.00   14.00    --  111.00  45.00 -60.00   63
 19  \w     79.00 136.00   1.00   14.00    --  111.00 178.00  60.00   57
 20  \w     71.00 103.00   1.00   14.00    --  111.00 -94.00  60.00   32
 21  \w     47.00  73.00   1.00   14.00    --  111.00 -61.00 150.00   26
 22  \w     76.00 102.00   1.00   14.00    --  111.00-111.00 150.00   26
 23  \w     60.00  87.00   1.00   14.00    --  111.00 -61.00  90.00   27
 24  \w     51.00  97.00   1.00   14.00    --  111.00-111.00 -60.00   46
 25  \w     54.00  80.00   1.00   14.00    --  111.00 -61.00-180.00   26
 26  \w     57.00  85.00   1.00   14.00    --  111.00-111.00  60.00   28
 27  \w      0.00  27.00   1.00    3.00    --  -41.52  37.00 -30.00   27
 28  \w      5.00  31.00   1.00    3.00    --  -41.52  19.00-150.00   26
 29  \w    -21.00  20.00   1.00    3.00    --  -41.52  37.00 120.00   41
 30  \w     11.00  37.00   1.00    3.00    --  -41.52  19.00-180.00   26
 31  \w     33.00  59.00   1.00    3.00    --   41.52-125.00 -60.00   26
 32  \w     25.00  64.00   1.00    3.00    --   41.52 -99.00  30.00   39
 33  \w     36.00  62.00   1.00    3.00    --   41.52-125.00 150.00   26
 34  \w    113.00 138.00   1.00   14.00    --  111.00  73.00-108.00   25
 35  \w     45.00  83.00   1.00   14.00    --  111.00-111.00-180.00   38
 36  \w    107.00 139.00   1.00   14.00    --  111.00  77.00  30.00   32
 37  \w     71.00 107.00   1.00   14.00    --  111.00 -94.00 120.00   36
 38  \w     84.00 159.00   1.00   14.00    --  111.00  61.00-180.00   75
 39  \w     69.00 108.00   1.00   14.00    --  111.00-111.00   0.00   39
 40  \w     40.00  65.00   1.00   14.00    --  111.00 -45.00  30.00   25
 41  \w    111.00 170.00   1.00   14.00    --  111.00 111.00 120.00   59
 42  \w     84.00 109.00   1.00   14.00    --  111.00-111.00-120.00   25
 43  \w     76.00 109.00   1.00   14.00    --  111.00-111.00  30.00   33
 44  \w     83.00 109.00   1.00   14.00    --  111.00-111.00  90.00   26
 45  \w    115.00 139.00   1.00   14.00    --  111.00 111.00   0.00   24
;
_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      0.0506075000
_diffrn_orient_matrix_UB_12      0.0517667000
_diffrn_orient_matrix_UB_13      0.0130226000
_diffrn_orient_matrix_UB_21      0.0059030000
_diffrn_orient_matrix_UB_22      -0.0379748000
_diffrn_orient_matrix_UB_23      0.0673868000
_diffrn_orient_matrix_UB_31      0.0365396000
_diffrn_orient_matrix_UB_32      -0.0654245000
_diffrn_orient_matrix_UB_33      -0.0289119000
_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  0.0478
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            84481
_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         76.377
_diffrn_reflns_theta_min         3.836
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.905
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43055
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             3280
_exptl_crystal_recrystallization_method
'Crystallised from concentrated benzene solution at room temperature'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.326(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     872
_refine_ls_number_reflns         16314
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0309
_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^)+(0.0298P)^2^+2.3037P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0747
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                15086
_reflns_number_total             16314
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00044k2.cif
_cod_data_source_block           063ljm23
_cod_depositor_comments
'Adding full bibliography for 7718002--7718016.cif.'
_cod_database_code               7718008
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C34 H64 Sr1 N3 Si4 K1 O1'
_shelx_estimated_absorpt_t_max   0.772
_shelx_estimated_absorpt_t_min   0.304
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.674(12)
 0.326(12)
2. 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
3. Restrained distances
 C48-C49B \\sim C48-C49A
 with sigma of 0.02
 C48-C50B \\sim C48-C50A
 with sigma of 0.02
 C14-C15B \\sim C14-C15A
 with sigma of 0.02
 C14-C16B \\sim C14-C16A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C49A \\sim C50A \\sim C49B \\sim C50B: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C15A \\sim C16A \\sim C15B \\sim C16B: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
5. Others
 Sof(H48A)=Sof(C49A)=Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(C50A)=Sof(H50A)=
 Sof(H50B)=Sof(H50C)=1-FVAR(1)
 Sof(H48)=Sof(C49B)=Sof(H49D)=Sof(H49E)=Sof(H49F)=Sof(C50B)=Sof(H50D)=
 Sof(H50E)=Sof(H50F)=FVAR(1)
 Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16A)=Sof(H16A)=
 Sof(H16B)=Sof(H16C)=1-FVAR(2)
 Sof(H14)=Sof(C15B)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16B)=Sof(H16D)=
 Sof(H16E)=Sof(H16F)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14), C14(H14A), C23(H23), C26(H26), C45(H45), C48(H48),
 C48(H48A), C57(H57), C60(H60)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C19(H19), C20(H20), C21(H21), C41(H41), C42(H42),
 C43(H43), C53(H53), C54(H54), C55(H55)
6.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), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C),
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29C,H29B), C30(H30A,H30C,
 H30B), C31(H31A,H31B,H31C), C32(H32A,H32C,H32B), C33(H33A,H33B,H33C), C34(H34A,
 H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C63(H63A,
 H63B,H63C), C64(H64A,H64C,H64B), C65(H65A,H65B,H65C), C66(H66A,H66C,H66B),
 C67(H67A,H67C,H67B), C68(H68A,H68B,H68C), C15A(H15A,H15B,H15C), C16A(H16A,H16B,
 H16C), C49A(H49A,H49B,H49C), C50A(H50A,H50B,H50C), C15B(H15D,H15E,H15F),
 C16B(H16D,H16E,H16F), C49B(H49D,H49E,H49F), C50B(H50D,H50E,H50F)
;
_shelx_res_checksum              47250
_shelx_hkl_checksum              90600
_ins_header
;
TITL 063ljm23_rint in Pnma 
REM Pnma (#62, found as Pmcn in cab setting)
CELL 1.54184  24.555459  16.811373  20.692995  90.0000  90.0000  90.0000
ZERR    8.00   0.000229   0.000152   0.000210   0.0000   0.0000   0.0000
LATT  1
SYMM -x+1/2,-y, z+1/2 
SYMM -x, y+1/2,-z 
SYMM  x+1/2,-y+1/2,-z+1/2 
SFAC C H N O Si K Sr
UNIT 384.00 512.00 24.00 8.00 32.00 8.00 8.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
TREF
HKLF 4
END
;
_olex2_exptl_crystal_mounting_method
'mounted on a MiTeGen MicroMount using perfluoropolyether oil and rapidly transferred to a goniometer head on a diffractometer fitted with an Oxford Cryostream open-flow nitrogen cooling device'
_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 1.549
_oxdiff_exptl_absorpt_empirical_full_min 0.568