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_4320764
_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            'C24 H48 Cl Cu N10 O4'
_chemical_formula_weight         639.71
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 104.458(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.122(2)
_cell_length_b                   11.7901(12)
_cell_length_c                   17.423(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      19.439
_cell_measurement_theta_min      17.512
_cell_volume                     3008.0(6)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
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_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5477
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_T_max  0.8814
_exptl_absorpt_correction_T_min  0.6529
_exptl_crystal_colour            FARBLOS
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       QUADER
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.217
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0794P)^2^+5.1090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1489
_reflns_number_gt                4368
_reflns_number_total             5265
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010563r_1.cif
_cod_data_source_block           vr03
_cod_original_cell_volume        3007.9(6)
_cod_database_code               4320764