Dependence of the Chemical Properties of Macrocyclic [NiII2L(μ-O2CR)]+ Complexes on the Basicity of the Carboxylato Coligands (L2-= macrocyclic N6S2ligand)
Ulrike Lehmann; Julia Klingele; Vasile Lozan; Gunther Steinfeld; Marco H. Klingele; Steffen Käss; Axel Rodenstein; Berthold Kersting; Inorganic Chemistry 49 (2010) 11018–11029; doi:10.1021/ic101574a

data_4317164
_publ_contact_author_address
; Institut fuer Anorganische Chemie
  Universitaet Leipzig, Johannisallee 29
  04103 Leipzig
  Germany
;
_publ_contact_author_email       b.kersting@uni-leipzig.de
_publ_contact_author_fax         '+49/(0)341/973 6199'
_publ_contact_author_name        'Prof. Dr Berthold Kersting'
_publ_contact_author_phone       '+49/(0)341/973 6143'
_publ_section_title
;
 Dependence of the Chemical Properties of Macrocyclic [NiII2L(\m-O2CR)]+
 Complexes on the Basicity of the Carboxylato Coligands (L2-= macrocyclic
 N6S2ligand)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11018
_journal_page_last               11029
_journal_paper_doi               10.1021/ic101574a
_journal_volume                  49
_journal_year                    2010
_chemical_compound_source
;
 Crystals were grown by slow evaporation from a mixed ethanol/
 acetonitrile solvent system
;
_chemical_formula_structural
; 
 [Ni2L(u-O2CCCH)][BPh4].1.5CH3CN 
;
_chemical_formula_sum            'C68 H89.5 B N7.5 Ni2 O2 S2'
_chemical_formula_weight         1236.32
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 112.26(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.208(4)
_cell_length_b                   18.136(4)
_cell_length_c                   20.086(4)
_cell_measurement_temperature    213(2)
_cell_volume                     6476(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  BRUKER-AXS
_diffrn_measurement_method       hemisphere
_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  0.1162
_diffrn_reflns_av_sigmaI/netI    0.2419
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            41077
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_T_max  0.8081
_exptl_absorpt_correction_T_min  0.7268
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pale-green
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2636
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.807
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         15584
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      0.807
_refine_ls_R_factor_all          0.2141
_refine_ls_R_factor_gt           0.0572
_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^)+(0.0587P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1678
_reflns_number_gt                5102
_reflns_number_total             15584
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101574a_si_001_4.cif
_cod_data_source_block           5
_cod_original_cell_volume        6476(2)
_cod_original_formula_sum        'C68 H89.50 B N7.50 Ni2 O2 S2'
_cod_database_code               4317164