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_4309727
_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         'C16 H33 Cu N3, C F3 O3 S'
_chemical_formula_sum            'C17 H33 Cu F3 N3 O3 S'
_chemical_formula_weight         480.06
_chemical_name_systematic
; 
 (acetonitrile-\kN)(N,N,N',N'-tetraethyl-(1R,2R)-trans-cyclohexanediamine-
\k^2^N,N')copper(I) trifluoromethanesulfonate 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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
_cell_angle_beta                 105.516(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1266(10)
_cell_length_b                   8.2904(10)
_cell_length_c                   13.9796(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      18.0
_cell_measurement_theta_min      9.5
_cell_volume                     1130.9(2)
_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, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0507
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2217
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.88
_diffrn_standards_decay_%        2.03
_diffrn_standards_interval_count 19
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.103
_exptl_absorpt_correction_T_max  0.802
_exptl_absorpt_correction_T_min  0.714
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_meas      1.41
_exptl_crystal_density_method    'neutral buoyancy in CCl4/hexane'
_exptl_crystal_description       needle
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_coef       0.012(2)
_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   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         2128
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+0.6008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1086
_reflns_number_gt                1834
_reflns_number_total             2128
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050331isi20050303_080925_6.cif
_cod_data_source_block           4a
_cod_original_cell_volume        1130.86(19)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4309727