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_7718009
_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         'C36 H62 Ca N2 O3 Si2'
_chemical_formula_sum            'C36 H62 Ca N2 O3 Si2'
_chemical_formula_weight         667.13
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   dual
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.5
_audit_creation_date             2024-06-12T13:47:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2024-12-18 deposited with the CCDC.	2025-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.4268(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.30216(17)
_cell_length_b                   20.9676(4)
_cell_length_c                   18.5303(3)
_cell_measurement_reflns_used    10340
_cell_measurement_temperature    120.01(11)
_cell_measurement_theta_max      72.247
_cell_measurement_theta_min      4.77
_cell_measurement_wavelength     1.54184
_cell_volume                     3995.60(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0856
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.9909
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0633947
_diffrn_orient_matrix_UB_12      -0.0580735
_diffrn_orient_matrix_UB_13      -0.0389463
_diffrn_orient_matrix_UB_21      -0.0863147
_diffrn_orient_matrix_UB_22      0.0449929
_diffrn_orient_matrix_UB_23      -0.0479267
_diffrn_orient_matrix_UB_31      0.1046776
_diffrn_orient_matrix_UB_32      0.0018902
_diffrn_orient_matrix_UB_33      -0.0559047
_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  0.0317
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27707
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        73.1113
_diffrn_reflns_theta_max         72.4363
_diffrn_reflns_theta_min         4.217
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.181
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.626
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
        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            colourless
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.297
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     487
_refine_ls_number_reflns         7859
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+1.3685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.0985
_reflns_Friedel_coverage         0
_reflns_number_gt                6876
_reflns_number_total             7859
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00044k2.cif
_cod_data_source_block           X23-AOR6-084a
_cod_depositor_comments
'Adding full bibliography for 7718002--7718016.cif.'
_cod_original_cell_volume        3995.62(12)
_cod_database_code               7718009
_shelx_shelxl_version_number     2019/3
_shelx_res_checksum              3980
_shelx_hkl_checksum              63699