An unusually stable octanuclear σ-mesityl-bridged µ4-oxo-copper(i) complex encapsulated by a pyrazolate-based compartmental ligand scaffold
Stollenz, Michael; Große, Christian; Meyer, Franc; Chemical Communications  (2008) 1744–1746; doi:10.1039/b717571j

data_7111517
_publ_section_title
;
 An unusually stable octanuclear \s-mesityl-bridged
 &#x00B5;4-oxo-copper(i) complex encapsulated by a pyrazolate-based
 compartmental ligand scaffold
;
_journal_issue                   15
_journal_name_full               'Chemical Communications'
_journal_page_first              1744
_journal_page_last               1746
_journal_paper_doi               10.1039/b717571j
_journal_year                    2008
_chemical_formula_moiety         '(C86 H98 Cu8 N12 O), 4.625(C4 H8 O)'
_chemical_formula_sum            'C104.5 H135 Cu8 N12 O5.625'
_chemical_formula_weight         2157.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.42(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.249(5)
_cell_length_b                   32.447(7)
_cell_length_c                   26.971(5)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      58.957
_cell_measurement_theta_min      2.7235
_cell_volume                     20328(7)
_computing_cell_refinement       'Bruker AXS SAINT (v 7.40A, Bruker 2006)'
_computing_data_collection       'Proteum2 (v 2.2-RC7, Bruker 2006)'
_computing_data_reduction        'Bruker AXS SAINT (v 7.40A, Bruker 2006)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (v 6.12)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.602
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker three circle diffractometer'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'mirror system'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0998
_diffrn_reflns_av_sigmaI/netI    0.0868
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            160032
_diffrn_reflns_theta_full        59.85
_diffrn_reflns_theta_max         59.85
_diffrn_reflns_theta_min         2.13
_diffrn_source                   'rotating anode'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.244
_exptl_absorpt_correction_T_max  0.9736
_exptl_absorpt_correction_T_min  0.3999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             8984
_exptl_crystal_recrystallization_method
'diffusion of diethyl ether into a THF solution'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.771
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.377
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2782
_refine_ls_number_reflns         29068
_refine_ls_number_restraints     1404
_refine_ls_restrained_S_all      1.365
_refine_ls_R_factor_all          0.1118
_refine_ls_R_factor_gt           0.0703
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+14.8445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1611
_refine_ls_wR_factor_ref         0.1767
_reflns_number_gt                18740
_reflns_number_total             29068
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b717571jsup1.cif
_cod_data_source_block           stollenz
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7111517