A Tris(pyrazolyl) η6-Arene Ligand That Selects Cu(I) over Cu(II)
Robert T. Stibrany; Chengmin Zhang; Thomas J. Emge; Harvey J. Schugar; Joseph A. Potenza; Spencer Knapp; Inorganic Chemistry 45 (2006) 9713–9720; doi:10.1021/ic060980+

data_4327309
_publ_contact_author
;
 Joseph A. Potenza
 Department of Chemistry and Chemical Biology
 Rutgers, The State University of New Jersey
 610 Taylor Road
 Piscataway, New Jersey 08854 USA 
;
_publ_contact_author_email       potenza@rutchem.rutgers.edu
_publ_contact_author_fax         '732 445 5312'
_publ_contact_author_phone       '732 445 2115'
_publ_section_title
;
 A Tris(pyrazolyl) \h6-Arene Ligand That Selects Cu(I) over Cu(II)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9713
_journal_page_last               9720
_journal_paper_doi               10.1021/ic060980+
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C36 H30 Cu N6, C F3 O3 S'
_chemical_formula_sum            'C37 H30 Cu F3 N6 O3 S'
_chemical_formula_weight         759.28
_chemical_name_common            '[Cu^I^4(trif)]^.^C6 H14'
_chemical_name_systematic
; 
 [(1,3,5-Tris[2'-((pyrazol-1-yl)methyl)
phenyl]benzene)copper(I)](trifluoromethanesulfonate)
 ^.^ hexane 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   12.7358(4)
_cell_length_b                   12.7358(4)
_cell_length_c                   44.271(3)
_cell_measurement_reflns_used    3740
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      51.728
_cell_measurement_theta_min      5.214
_cell_volume                     6218.7(5)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics
'ORTEPIII (Burnett & Johnson, 1996), ORTEP32 (Farrugia, 1997)'
_computing_publication_material  'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0874
_diffrn_reflns_av_sigmaI/netI    0.0579
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            16198
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.90
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.630
_exptl_absorpt_correction_T_max  0.9514
_exptl_absorpt_correction_T_min  0.9283
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Blessing, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             2340
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_platon_squeeze_details
; 
 The structure contained highly disordered hexane in the 
 asymmetric unit; because refinement of the hexane molecules led 
 to unrealistic geometric parameters, even with the use of 
 constraints, a structural model was refined with contributions 
 from the hexane molecules removed from the diffraction data by 
 using the SQUEEZE algorithm in PLATON (Spek, 1990).  
;
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         2358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0408P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0869
_reflns_number_gt                1805
_reflns_number_total             2358
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic0609802Bsi20060919_023840_2.cif
_cod_data_source_block           Cu(4)(trif)
_cod_original_cell_volume        6218.8(5)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4327309