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_7717532
_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         'C122 H106 Cu8 N14 O24 Si10, 2(C3 H7 N O)'
_chemical_formula_sum            'C128 H120 Cu8 N16 O26 Si10'
_chemical_formula_weight         3087.71
_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
;
2024-10-13 deposited with the CCDC.	2024-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                89.5344(10)
_cell_angle_beta                 87.6687(10)
_cell_angle_gamma                71.8144(12)
_cell_formula_units_Z            2
_cell_length_a                   19.0322(3)
_cell_length_b                   19.1168(3)
_cell_length_c                   19.7780(2)
_cell_measurement_reflns_used    46456
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.587
_cell_measurement_theta_min      2.197
_cell_volume                     6830.75(17)
_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 0.996
_diffrn_measured_fraction_theta_max 0.967
_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  0.0586
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            112915
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.279
_diffrn_reflns_theta_min         2.236
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.803
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.684
_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    1.501
_exptl_crystal_description       prism
_exptl_crystal_F_000             3160
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.535
_refine_diff_density_min         -1.163
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1629
_refine_ls_number_reflns         28936
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0966P)^2^+11.468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1554
_refine_ls_wR_factor_ref         0.1633
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24569
_reflns_number_total             28936
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02690j3.cif
_cod_data_source_block           1b
_cod_depositor_comments
'Adding full bibliography for 7717529--7717532.cif.'
_cod_database_code               7717532
_shelx_estimated_absorpt_t_min   0.578
_shelx_estimated_absorpt_t_max   0.712
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2013-4
_shelx_res_checksum              10692
_shelx_fab_checksum              86648