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_7717530
_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         'C96 H76 Cu8 N4 O26 Si10'
_chemical_formula_sum            'C96 H76 Cu8 N4 O26 Si10'
_chemical_formula_weight         2490.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2024-08-05 deposited with the CCDC.	2024-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.432(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.8329(16)
_cell_length_b                   16.5280(15)
_cell_length_c                   20.4641(19)
_cell_measurement_reflns_used    1000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.2
_cell_measurement_theta_min      2.6
_cell_volume                     5785.3(10)
_computing_cell_refinement       'iMosflm (Battye et al., 2011)'
_computing_data_collection       'Marccd (Doyle, 2011)'
_computing_data_reduction        iMosflm
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2015)'
_computing_publication_material  SHELXTL
_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 0.981
_diffrn_measurement_device_type  'Rayonix SX-165 CCD'
_diffrn_measurement_method       '/f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.74500
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            86211
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        26.551
_diffrn_reflns_theta_max         31.002
_diffrn_reflns_theta_min         2.530
_exptl_absorpt_coefficient_mu    1.830
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scala (Evans, 2006)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_description       prism
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.592
_refine_diff_density_min         -1.308
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.0042(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         15724
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1320
_refine_ls_R_factor_gt           0.0761
_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^)+(0.08P)^2^+10P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1819
_refine_ls_wR_factor_ref         0.2159
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8805
_reflns_number_total             15724
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02690j3.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7717529--7717532.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7717530
_shelx_estimated_absorpt_t_min   0.854
_shelx_estimated_absorpt_t_max   0.948
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2013-4
_shelx_res_checksum              77189
_shelx_fab_checksum              62847