An ionic Cu<sub>9</sub>Na<sub>4</sub>-phenylsilsesquioxane/bis(triphenylphosphine)iminium complex: synthesis, unique structure, and catalytic activity.
Bilyachenko, Alexey N.; Khrustalev, Victor N.; Huang, Zhibin; Dubinina, Kristina D.; Shubina, Elena S.; Lobanov, Nikolai N.; Sun, Di; Alegria, Elisabete C. B. A.; Pombeiro, Armando J. L.; Nanoscale 16 (2024) 19266–19275; doi:10.1039/d4nr02298j

data_1572729
_publ_section_title
;
 An ionic
 Cu<sub>9</sub>Na<sub>4</sub>-phenylsilsesquioxane/bis(triphenylphosphine)iminium
 complex: synthesis, unique structure, and catalytic activity.
;
_journal_issue                   41
_journal_name_full               Nanoscale
_journal_page_first              19266
_journal_page_last               19275
_journal_paper_doi               10.1039/d4nr02298j
_journal_volume                  16
_journal_year                    2024
_chemical_formula_moiety
'C128 H124 Cu9 Na4 O46 Si20, 2(C36 H30 N P2), 3.5(C2 H6 O)'
_chemical_formula_sum            'C207 H205 Cu9 N2 Na4 O49.5 P4 Si20'
_chemical_formula_weight         4862.33
_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-2013
_audit_update_record
;
2024-05-05 deposited with the CCDC.	2024-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                75.3941(12)
_cell_angle_beta                 87.8609(13)
_cell_angle_gamma                89.5919(12)
_cell_formula_units_Z            2
_cell_length_a                   16.3354(9)
_cell_length_b                   24.6172(13)
_cell_length_c                   28.7146(15)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.04
_cell_measurement_theta_min      2.45
_cell_volume                     11166.1(10)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX3 (Bruker, 2018)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON-III CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1153
_diffrn_reflns_av_unetI/netI     0.1140
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            151409
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         2.023
_exptl_absorpt_coefficient_mu    1.058
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_correction_T_min  0.876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10. 
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       prism
_exptl_crystal_F_000             5004
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.694
_refine_diff_density_min         -1.071
_refine_diff_density_rms         0.139
_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     1765
_refine_ls_number_reflns         41427
_refine_ls_number_restraints     696
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1898
_refine_ls_R_factor_gt           0.1034
_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^)+(0.01P)^2^+120.P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2066
_refine_ls_wR_factor_ref         0.2383
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20771
_reflns_number_total             41427
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr02298j2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 1572729.cif.'
_cod_original_formula_sum        'C207 H205 Cu9 N2 Na4 O49.50 P4 Si20'
_cod_database_code               1572729
_shelx_estimated_absorpt_t_min   0.884
_shelx_estimated_absorpt_t_max   0.939
_shelxl_version_number           2013-4
_shelx_res_checksum              29401
_shelx_hkl_checksum              90973