In situ hydrothermal synthesis of dysprosium(iii) single-molecule magnet with lanthanide salt as catalyst
Liang, Li; Peng, Guo; Li, Guizhu; Lan, Yanhua; Powell, Annie K.; Deng, Hong; Dalton Transactions 41 (2012) 5816–; doi:10.1039/c2dt30175j

data_7018973
_publ_section_title
;
 In situ hydrothermal synthesis of dysprosium(iii) single-molecule magnet
 with lanthanide salt as catalyst
;
_journal_issue                   19
_journal_name_full               'Dalton Transactions'
_journal_page_first              5816
_journal_paper_doi               10.1039/c2dt30175j
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C32 H34 N16 O16 Tb2, 4(H2 O)'
_chemical_formula_sum            'C32 H42 N16 O20 Tb2'
_chemical_formula_weight         1288.68
_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                117.2750(10)
_cell_angle_beta                 98.1120(10)
_cell_angle_gamma                99.4350(10)
_cell_formula_units_Z            1
_cell_length_a                   9.1459(18)
_cell_length_b                   11.9522(10)
_cell_length_c                   12.1423(10)
_cell_measurement_reflns_used    3974
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.19
_cell_measurement_theta_min      1.95
_cell_volume                     1127.8(3)
_computing_cell_refinement       'Apex2 (Bruker, 2005)'
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        'Apex2 (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL 6.12'
_computing_publication_material  'SHELXTL 6.12'
_computing_structure_refinement  'SHELXTL 6.12'
_computing_structure_solution    'SHELXTL 6.12 (Bruker, 2000-2003)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       '\w scans'
_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  0.0146
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5802
_diffrn_reflns_theta_full        25.19
_diffrn_reflns_theta_max         25.19
_diffrn_reflns_theta_min         1.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.206
_exptl_absorpt_correction_T_max  0.5019
_exptl_absorpt_correction_T_min  0.4471
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.897
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             636.0
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         3974
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0210
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0227P)^2^+0.9385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0498
_reflns_number_gt                3744
_reflns_number_total             3974
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30175j.txt
_cod_data_source_block           4
_cod_database_code               7018973