Stepwise azido transfer to cerous tris(<i>tert</i>-butoxy)siloxide <i>via</i> trans-silylation with Me<sub>3</sub>SiN<sub>3</sub>.
Friedrich, Jochen; Riedmaier, Jonas; Maichle-Mössmer, Cäcilia; Anwander, Reiner; Dalton transactions (Cambridge, England : 2003) 54 (2025) 12141–12144; doi:10.1039/d5dt01051a

data_7719121
_publ_section_title
;
 Stepwise azido transfer to cerous tris(<i>tert</i>-butoxy)siloxide
 <i>via</i> trans-silylation with Me<sub>3</sub>SiN<sub>3</sub>.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12141
_journal_page_last               12144
_journal_paper_doi               10.1039/d5dt01051a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_sum            'C66 H149 Ce2 N3 O20 Si5'
_chemical_formula_weight         1725.56
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2025-05-02 deposited with the CCDC.	2025-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                106.406(2)
_cell_angle_beta                 94.011(2)
_cell_angle_gamma                100.800(2)
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_cell_length_b                   25.3201(16)
_cell_length_c                   26.9650(15)
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.87
_cell_measurement_theta_min      2.274
_cell_volume                     9061.1(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1316
_diffrn_reflns_av_unetI/netI     0.1509
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            137029
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.492
_diffrn_reflns_theta_min         1.334
_diffrn_source                   'ImuS-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.117
_exptl_absorpt_correction_T_max  0.9680
_exptl_absorpt_correction_T_min  0.7430
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_description       plate
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.269
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.028
_refine_diff_density_max         1.369
_refine_diff_density_min         -1.700
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1913
_refine_ls_number_reflns         36857
_refine_ls_number_restraints     1323
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.1327
_refine_ls_R_factor_gt           0.0609
_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^)+(0.0467P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1348
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21254
_reflns_number_total             36857
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01051a2.cif
_cod_data_source_block           1_mo_jfr185Ba_0m
_cod_depositor_comments
'Adding full bibliography for 7719121--7719122.cif.'
_cod_database_code               7719121
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.753
_shelx_estimated_absorpt_t_max   0.969
_shelx_res_checksum              66845
_shelx_hkl_checksum              44735