An octanuclear 3-phenyl-5-(2-pyridyl)pyrazolate/phenylsilsesquioxane complex: synthesis, unique structure, and catalytic activity.
Bilyachenko, Alexey N.; Khrustalev, Victor N.; Huang, Zhibin; Shul'pina, Lidia S.; Dorovatovskii, Pavel V.; Shubina, Elena S.; Ikonnikov, Nikolay S.; Lobanov, Nikolai N.; Ragimov, Karim; Sun, Di; Dalton transactions (Cambridge, England : 2003) 53 (2024) 19102–19106; doi:10.1039/d4dt02690j

data_7717531
_publ_section_title
;
 An octanuclear 3-phenyl-5-(2-pyridyl)pyrazolate/phenylsilsesquioxane
 complex: synthesis, unique structure, and catalytic activity.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19102
_journal_page_last               19106
_journal_paper_doi               10.1039/d4dt02690j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C120 H100 Cu8 N12 O22 Si10'
_chemical_formula_sum            'C120 H100 Cu8 N12 O22 Si10'
_chemical_formula_weight         2851.43
_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
;
2024-09-05 deposited with the CCDC.	2024-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                64.6067(17)
_cell_angle_beta                 89.6243(14)
_cell_angle_gamma                79.3532(14)
_cell_formula_units_Z            1
_cell_length_a                   12.3924(2)
_cell_length_b                   17.2730(3)
_cell_length_c                   17.8005(3)
_cell_measurement_reflns_used    47616
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.87
_cell_measurement_theta_min      2.75
_cell_volume                     3371.53(11)
_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 0.983
_diffrn_measured_fraction_theta_max 0.977
_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  0.0683
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            85875
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.939
_diffrn_reflns_theta_min         2.891
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.761
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.134a (Rigaku Oxford Diffraction, 2024).
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_description       prism
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.231
_refine_diff_density_min         -1.054
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     777
_refine_ls_number_reflns         14369
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1233
_refine_ls_R_factor_gt           0.1178
_refine_ls_shift/su_max          0.000
_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^+90P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2716
_refine_ls_wR_factor_ref         0.2738
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12926
_reflns_number_total             14369
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02690j3.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 7717529--7717532.cif.'
_cod_database_code               7717531
_shelx_estimated_absorpt_t_min   0.715
_shelx_estimated_absorpt_t_max   0.789
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2013-4
_shelx_res_checksum              78593
_shelx_fab_checksum              53637