Synthesis and Structures of Cuprous Triptycylthiolate Complexes
Skylar J. Ferrara; Joel T. Mague; James P. Donahue; Inorganic Chemistry 51 (2012) 6567–6576; doi:10.1021/ic300124n

data_4329442
_publ_contact_author             'James P. Donahue'
_publ_contact_author_address
;
   James P. Donahue
   Department of Chemistry
   Tulane University
   Percival Stern Hall, Room 2015
   6400 Freret Street
   New Orleans, Louisiana 70118-5698
;
_publ_contact_author_email       donahue@tulane.edu
_publ_section_title
;
 Synthesis and Structures of Cuprous Triptycylthiolate Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6567
_journal_page_last               6576
_journal_paper_doi               10.1021/ic300124n
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C40 H26 Cu S2, C16 H36 N, C4 H10 O'
_chemical_formula_sum            'C60 H72 Cu N O S2'
_chemical_formula_weight         950.85
_chemical_name_systematic
; 
 Tetra(n-butyl)ammonium bis(tryptcylthiolato)cuprate(I) 
diethyl ether solvate 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.892(1)
_cell_angle_beta                 105.633(1)
_cell_angle_gamma                108.445(1)
_cell_formula_units_Z            2
_cell_length_a                   11.5110(7)
_cell_length_b                   16.0819(10)
_cell_length_c                   16.7584(11)
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.50
_cell_volume                     2703.4(3)
_computing_cell_refinement       'Bruker SAINT (Bruker-AXS 2009)'
_computing_data_collection       'Bruker APEX2 (Bruker-AXS, 2010)'
_computing_data_reduction        'Bruker SAINT (Bruker-AXS 2009)'
_computing_molecular_graphics    'Bruker SHELXTL(Bruker-AXS 2008)'
_computing_publication_material  'Bruker SHELXTL(Bruker-AXS 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_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  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0532
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            47339
_diffrn_reflns_theta_full        27.751
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.520
_exptl_absorpt_correction_T_max  0.9223
_exptl_absorpt_correction_T_min  0.6876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008a)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_description       Column
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_platon_squeeze_details
; 
A badly disordered molecule of THF was removed with the 
SQUEEZE option of the PLATON package (Spek, 2010). 
;
_refine_diff_density_max         1.831
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         13166
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1136P)^2^+0.7565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1828
_refine_ls_wR_factor_ref         0.1968
_reflns_number_gt                9277
_reflns_number_total             13166
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300124n_si_003_08.cif
_cod_data_source_block           jpd425_0m
_cod_database_code               4329442