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_4309726
_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
'C24 H52 Cu2 N4 O2, 2(C F3 O3 S), 4(C H2 Cl2)'
_chemical_formula_sum            'C30 H60 Cl8 Cu2 F6 N4 O8 S2'
_chemical_formula_weight         1193.62
_chemical_name_systematic
; 
 di-\m-oxo-bis(N,N'-diethyl-N,N'-dimethyl-(1R,2R)-trans-cyclohexanediamine-
\k^2^N,N')copper(III) bis(trifluoromethanesulfonate) dichloromethane solvate 
;
_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                 108.387(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.1336(2)
_cell_length_b                   11.9387(3)
_cell_length_c                   18.4717(3)
_cell_measurement_reflns_used    6569
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      23.66
_cell_measurement_theta_min      1.16
_cell_volume                     2539.19(9)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'Siemens SAINT (Siemens, 1995)'
_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      143(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Siemens SMART CCD'
_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    0.0699
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6447
_diffrn_reflns_theta_full        23.66
_diffrn_reflns_theta_max         23.66
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    1.408
_exptl_absorpt_correction_T_max  0.870
_exptl_absorpt_correction_T_min  0.715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'XPREP: (v 5.03) Siemens Industrial Automation, Inc.: Madison, WI (1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.875
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(2)
_refine_ls_extinction_coef       0.0022(3)
_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   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         6446
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0137P)^2^+10.5184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1287
_reflns_number_gt                5722
_reflns_number_total             6446
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050331isi20050303_080925_5.cif
_cod_data_source_block           3b
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4309726