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_7025391
_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 N12 O50 Y4, 2(N O3), 7(H2 O), 6(C H4 O)'
_chemical_formula_sum            'C52 H136 Co6 N14 O69 Y4'
_chemical_formula_weight         2770.97
_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                72.353(2)
_cell_angle_beta                 70.913(2)
_cell_angle_gamma                72.982(2)
_cell_formula_units_Z            1
_cell_length_a                   12.7727(14)
_cell_length_b                   13.6246(15)
_cell_length_c                   16.6712(18)
_cell_measurement_reflns_used    6811
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.98
_cell_measurement_theta_min      2.31
_cell_volume                     2551.6(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 0.994
_diffrn_measured_fraction_theta_max 0.897
_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  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19033
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    3.310
_exptl_absorpt_correction_T_max  0.506
_exptl_absorpt_correction_T_min  0.393
_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    1.803
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.240
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         11005
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0553
_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^)+(0.0931P)^2^+5.6116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1483
_refine_ls_wR_factor_ref         0.1634
_reflns_number_gt                8185
_reflns_number_total             11005
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c000008f.txt
_cod_data_source_block           hua416
_cod_database_code               7025391