High-nuclearity Cu<sub>14</sub> ionic complex featuring 1,3-bis(diphenylphosphino)propane and methylsilsesquioxane ligands: highly efficient catalysis of mild peroxidative alkane fuctionalizations.
Arteev, Ivan S.; Khrustalev, Victor N.; Shul'pina, Lidia S.; Rodionov, Alexey N.; Shubina, Elena S.; Ragimov, Karim; Wang, Zhi; Bilyachenko, Alexey N.; Chemical communications (Cambridge, England)  (2025) –; doi:10.1039/d5cc05805h

data_7135248
_publ_section_title
;
 High-nuclearity Cu<sub>14</sub> ionic complex featuring
 1,3-bis(diphenylphosphino)propane and methylsilsesquioxane ligands:
 highly efficient catalysis of mild peroxidative alkane fuctionalizations.
;
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/d5cc05805h
_journal_year                    2025
_chemical_formula_moiety
'C16.10 H48.90 Cl0.90 Cu12 O37.20 Si16, 2(C54 H52 Cu P4), 2(C H Cl3)'
_chemical_formula_sum            'C126.1 H154.9 Cl6.9 Cu14 O37.2 P8 Si16'
_chemical_formula_weight         4097.31
_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   mixed
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/2
_audit_update_record
;
2025-10-10 deposited with the CCDC.	2025-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                94.8170(10)
_cell_angle_beta                 94.5880(10)
_cell_angle_gamma                94.8450(10)
_cell_formula_units_Z            1
_cell_length_a                   14.2336(2)
_cell_length_b                   16.6267(2)
_cell_length_c                   18.4779(2)
_cell_measurement_reflns_used    33565
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      78.840
_cell_measurement_theta_min      2.693
_cell_volume                     4325.19(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2015)'
_computing_publication_material  'SHELXTL (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type
'Rigaku XtaLAB Synergy-S, HyPix-6000HE area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0867
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            90576
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.794
_diffrn_reflns_theta_min         2.409
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    5.108
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.137a (Rigaku Oxford Diffraction, 2024).
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       plate
_exptl_crystal_F_000             2076
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.158
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     957
_refine_ls_number_reflns         18503
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0635
_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^)+(0.099P)^2^+9P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1612
_refine_ls_wR_factor_ref         0.1733
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15129
_reflns_number_total             18503
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc05805h2.cif
_cod_data_source_block           ISA344
_cod_original_formula_sum        'C126.10 H154.90 Cl6.90 Cu14 O37.20 P8 Si16'
_cod_database_code               7135248
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.399
_shelx_estimated_absorpt_t_max   0.905
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              13332
_shelx_hkl_checksum              28440
_shelx_fab_checksum              21554