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_7001447
_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(C38 H38 Cl2 Cu2 N6), 4(F6 P), C H2 Cl2'
_chemical_formula_sum            'C77 H78 Cl6 Cu4 F24 N12 P4'
_chemical_formula_weight         2218.29
_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                90.000
_cell_angle_beta                 115.575(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   13.347(2)
_cell_length_b                   14.191(2)
_cell_length_c                   14.720(2)
_cell_measurement_reflns_used    221
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.46
_cell_measurement_theta_min      3.17
_cell_volume                     2514.9(7)
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Schakal-99 (E.Keller 1999)'
_computing_publication_material  'XCIF 6.12 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.1935
_diffrn_reflns_av_sigmaI/netI    0.1156
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18022
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    1.147
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS version 2.03.(Sheldrick,Bruker AXS Inc.'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1118
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3139
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.1653
_refine_ls_R_factor_gt           0.0877
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1590P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2205
_refine_ls_wR_factor_ref         0.2584
_reflns_number_gt                1597
_reflns_number_total             3139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b901832h.txt
_cod_data_source_block           bamono
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        ' C77 H78 Cl6 Cu4 F24 N12 P4 '
_cod_database_code               7001447