Novel mixed-valent CoII2CoIII4LnIII4 aggregates with ligands derived from tris-(hydroxymethyl)aminomethane (Tris)
Xiang, Hua; Lan, Yanhua; Li, Huan-Yong; Jiang, Long; Lu, Tong-Bu; Anson, Christopher E.; Powell, Annie K.; Dalton Transactions 39 (2010) 4737–; doi:10.1039/c000008f

data_7025393
_publ_section_title
;
 Novel mixed-valent CoII2CoIII4LnIII4 aggregates with ligands derived from
 tris-(hydroxymethyl)aminomethane (Tris)
;
_journal_issue                   20
_journal_name_full               'Dalton Transactions'
_journal_page_first              4737
_journal_paper_doi               10.1039/c000008f
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety
'C46 H98 Co6 Dy4 N12 O50, 2(N O3), 6(H2 O), 4(C H4 O)'
_chemical_formula_sum            'C50 H126 Co6 Dy4 N14 O66'
_chemical_formula_weight         2983.23
_chemical_name_systematic
;
?
;
_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                72.386(2)
_cell_angle_beta                 71.502(2)
_cell_angle_gamma                73.644(2)
_cell_formula_units_Z            1
_cell_length_a                   12.8569(15)
_cell_length_b                   13.6424(16)
_cell_length_c                   16.3608(19)
_cell_measurement_reflns_used    10112
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.98
_cell_measurement_theta_min      2.43
_cell_volume                     2538.5(5)
_computing_cell_refinement       'SMART-NT 5.6 (Bruker AXS Inc., 2005)'
_computing_data_collection       'SMART-NT 5.6 (Bruker AXS Inc., 2005)'
_computing_data_reduction        'SAINT+ 6.45 (Bruker AXS Inc., 2003)'
_computing_molecular_graphics    'Diamond 2.1 (Crystal Impact, 1998)'
_computing_publication_material  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_refinement  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_solution    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_device_type  'Bruker SMART Apex'
_diffrn_measurement_method       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17186
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    3.968
_exptl_absorpt_correction_T_max  0.539
_exptl_absorpt_correction_T_min  0.315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Bruker AXS Inc., 2005)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.951
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1478
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         5.874
_refine_diff_density_min         -2.605
_refine_diff_density_rms         0.300
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         10754
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0615
_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^)+(0.1178P)^2^+13.5861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1669
_refine_ls_wR_factor_ref         0.1899
_reflns_number_gt                8149
_reflns_number_total             10754
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c000008f.txt
_cod_data_source_block           hua374
_cod_database_code               7025393