Bis(μ-oxo)dicopper(III) Complexes of a Homologous Series of Simple Peralkylated 1,2-Diamines: Steric Modulation of Structure, Stability, and Reactivity
Adam P. Cole; Viswanath Mahadevan; Liviu M. Mirica; Xavier Ottenwaelder; T. Daniel P. Stack; Inorganic Chemistry 44 (2005) 7345–7364; doi:10.1021/ic050331i

data_4309723
_publ_section_title
;
Bis(\m-oxo)dicopper(III) Complexes of a Homologous Series of Simple
Peralkylated 1,2-Diamines: Steric Modulation of Structure, Stability, and
Reactivity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7345
_journal_page_last               7364
_journal_paper_doi               10.1021/ic050331i
_journal_volume                  44
_journal_year                    2005
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C28 H37 Cu N2 P, C F3 O3 S'
_chemical_formula_sum            'C29 H37 Cu F3 N2 O3 P S'
_chemical_formula_weight         645.21
_chemical_name_systematic
; 
 (triphenylphosphine-\kP)(N,N,N',N'-tetramethyl-(1R,2R)-trans-
cyclohexanediamine-\k^2^N,N')copper(I) trifluoromethanesulfonate 
;
_space_group_IT_number           1
_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                68.4860(70)
_cell_angle_beta                 74.8550(50)
_cell_angle_gamma                67.0250(70)
_cell_formula_units_Z            1
_cell_length_a                   8.1394(10)
_cell_length_b                   9.0186(10)
_cell_length_c                   12.2394(10)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      17.5
_cell_volume                     762.19(15)
_computing_cell_refinement       'Enraf-Nonius CAD4 Express'
_computing_data_collection       'Enraf-Nonius CAD4 Express'
_computing_data_reduction        'Enraf-Nonius CAD4 Express'
_computing_molecular_graphics
'Ortep-3 for Windows: LJ Farrugia, J. Appl. Cryst (1997), 30, 565'
_computing_publication_material
'CIFTAB, Sheldrick 1993; CRYSTAL MS Word Macro; Adam Cole 2003'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0177
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2862
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        1.5
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.888
_exptl_absorpt_correction_T_max  0.770
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_meas      1.40
_exptl_crystal_density_method    'neutral buoyancy in CCl4/hexane'
_exptl_crystal_description       'rhombic block'
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.002(10)
_refine_ls_extinction_coef       0.080(5)
_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   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         2862
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.2208P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0756
_reflns_number_gt                2811
_reflns_number_total             2862
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050331isi20050303_080925_2.cif
_cod_data_source_block           1d
_cod_database_code               4309723