Structural Comparison of Copper(I) and Copper(II) Complexes with Tris(2-pyridylmethyl)amine Ligand
William T. Eckenhoff; Tomislav Pintauer; Inorganic Chemistry 49 (2010) 10617–10626; doi:10.1021/ic1016142

data_4317052
_publ_section_title
;
 Structural Comparison of Copper(I) and Copper(II) Complexes with
 Tris(2-pyridylmethyl)amine Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10617
_journal_page_last               10626
_journal_paper_doi               10.1021/ic1016142
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C24 H20 B, C18 H18 Cu N4'
_chemical_formula_sum            'C42 H38 B Cu N4'
_chemical_formula_weight         673.11
_space_group_IT_number           2
_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                89.620(5)
_cell_angle_beta                 81.377(5)
_cell_angle_gamma                79.961(5)
_cell_formula_units_Z            4
_cell_length_a                   11.552(4)
_cell_length_b                   13.797(5)
_cell_length_c                   21.629(7)
_cell_measurement_reflns_used    5913
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.350
_cell_measurement_theta_min      2.139
_cell_volume                     3355(2)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2000)'
_computing_publication_material  'ORTEP-3 for Windows (Faruggia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker Smart ApexII'
_diffrn_measurement_method       '\f and \w 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  0.0686
_diffrn_reflns_av_sigmaI/netI    0.0919
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26263
_diffrn_reflns_theta_full        25.17
_diffrn_reflns_theta_max         25.17
_diffrn_reflns_theta_min         0.95
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         11912
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  0.8468
_exptl_absorpt_correction_T_min  0.7800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhomboid
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.511
_refine_diff_density_min         -1.226
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         11912
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1275P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1747
_refine_ls_wR_factor_ref         0.2042
_reflns_number_gt                8002
_reflns_number_total             11912
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1016142_si_002_02.cif
_cod_data_source_block           '[Cu(TPMA)][BPh4]'
_cod_original_cell_volume        3355.6(19)
_cod_database_code               4317052