Copper Complexes of Novel Superbasic Peralkylguanidine Derivatives of Tris(2-aminoethyl)amine as Constraint Geometry Ligands
Volker Raab; Jennifer Kipke; Olaf Burghaus; Jörg Sundermeyer; Inorganic Chemistry 40 (2001) 6964–6971; doi:10.1021/ic010563r

data_4320765
_publ_contact_author
;
         Joerg Sundermeyer
         Fachbereich Chemie der Universit\"at
         Philipps Universit\"at Marburg
         Hans-Meerwein-Str.
         35032 Marburg
         Bundesrepublik Deutschland
;
_publ_contact_author_email       jsu@chemie.uni-marburg.de
_publ_contact_author_fax         '+49 6421 2828917 '
_publ_contact_author_phone       '+49 6421 2825693 '
_publ_section_title
;
 Copper Complexes of Novel Superbasic Peralkylguanidine Derivatives of
 Tris(2-aminoethyl)amine as Constraint Geometry Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6964
_journal_page_last               6971
_journal_paper_doi               10.1021/ic010563r
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C23 H51 Cl2 Cu N11 O8'
_chemical_formula_weight         744.19
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.194(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.080(2)
_cell_length_b                   13.2459(13)
_cell_length_c                   16.367(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      14.522
_cell_measurement_theta_min      11.194
_cell_volume                     3476.7(8)
_computing_cell_refinement       'CAD4 EXPRESS'
_computing_data_collection       'CAD4 EXPRESS'
_computing_data_reduction        'XCAD4 (Harms, 1997)'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(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       Omega-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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6641
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.40
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.841
_exptl_absorpt_correction_T_max  0.8842
_exptl_absorpt_correction_T_min  0.4319
_exptl_crystal_colour            DUNKELGRUEN
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       QUADER
_exptl_crystal_F_000             1572
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.626
_refine_diff_density_min         -1.349
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         6091
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0618
_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^)+(0.0940P)^2^+11.4014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1837
_refine_ls_wR_factor_ref         0.2073
_reflns_number_gt                5019
_reflns_number_total             6091
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010563r_2.cif
_cod_data_source_block           vr04
_cod_original_cell_volume        3476.7(9)
_cod_database_code               4320765