Interaction of an extended series of N-substituted di(2-picolyl)amine derivatives with copper(II). Synthetic, structural, magnetic and solution studies
Antonioli, Bianca; Büchner, Bernd; Clegg, Jack K.; Gloe, Kerstin; Gloe, Karsten; Götzke, Linda; Heine, Axel; Jäger, Anne; Jolliffe, Katrina A.; Kataeva, Olga; Kataev, Vladislav; Klingeler, Rüdiger; Krause, Tilo; Lindoy, Leonard F.; Popa, Andreia; Seichter, Wilhelm; Wenzel, Marco; Dalton Transactions  (2009) 4795–4805; doi:10.1039/b901832h

data_7001448
_publ_section_title
;
 Interaction of an extended series of N-substituted di(2-picolyl)amine
 derivatives with copper(II). Synthetic, structural, magnetic and
 solution studies
;
_journal_issue                   24
_journal_name_full               'Dalton Transactions'
_journal_page_first              4795
_journal_page_last               4805
_journal_paper_doi               10.1039/b901832h
_journal_year                    2009
_chemical_formula_moiety         '2(C27 H25 Cl2 Cu N3 O9),(H2 O)'
_chemical_formula_sum            'C54 H52 Cl4 Cu2 N6 O19'
_chemical_formula_weight         1357.90
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 99.343(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.1257(3)
_cell_length_b                   10.5924(2)
_cell_length_c                   36.7101(6)
_cell_measurement_reflns_used    2521
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.25
_cell_measurement_theta_min      2.56
_cell_volume                     5419.89(18)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker Smart Apex 2 CCD '
_diffrn_measurement_method       '\f and \w scan'
_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  0.0734
_diffrn_reflns_av_sigmaI/netI    0.0913
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            118862
_diffrn_reflns_theta_full        31.56
_diffrn_reflns_theta_max         31.56
_diffrn_reflns_theta_min         1.12
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.067
_exptl_absorpt_correction_T_max  0.808
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick,1999-2003)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.169
_refine_diff_density_min         -0.972
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         17776
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.1027
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0256P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.0964
_reflns_number_gt                9736
_reflns_number_total             17776
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b901832h.txt
_cod_data_source_block           gloe1a
_cod_original_cell_volume        5419.88(18)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7001448