The synthesis of a 3d‒4f polynuclear metal cluster under microwave irradiation: crystal structure and magnetic property of [La3Ni6(IDA)6(OH)6(H2O)12]·3NO3·15H2O (IDA = iminodiacetate)
Zhuang, Gui-Lin; Sun, Xiao-Jun; Long, La-Sheng; Huang, Rong-Bin; Zheng, Lan-Sun; Dalton Transactions  (2009) 4640–4642; doi:10.1039/b823294f

data_7001454
_publ_section_title
;
 The synthesis of a 3d--4f polynuclear metal cluster under microwave
 irradiation: crystal structure and magnetic property of
 [La3Ni6(IDA)6(OH)6(H2O)12]&#x00B7;3NO3&#x00B7;15H2O (IDA =
 iminodiacetate)
;
_journal_issue                   24
_journal_name_full               'Dalton Transactions'
_journal_page_first              4640
_journal_page_last               4642
_journal_paper_doi               10.1039/b823294f
_journal_year                    2009
_chemical_formula_moiety         '[La3Ni6(C4H5O4N)6(OH)6(H2O)12].3(NO3).15(H2O)'
_chemical_formula_sum            'C24 H90 La3 N9 Ni6 O66'
_chemical_formula_weight         2330.04
_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                77.8360(10)
_cell_angle_beta                 82.1800(10)
_cell_angle_gamma                80.6840(10)
_cell_formula_units_Z            2
_cell_length_a                   12.8557(2)
_cell_length_b                   15.9543(3)
_cell_length_c                   18.2385(3)
_cell_measurement_reflns_used    35832
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.6209
_cell_measurement_theta_min      2.4115
_cell_volume                     3588.36(11)
_computing_cell_refinement       'CrysAlis RED'
_computing_data_collection       'CrysAlis CCD'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CrysAlis CCD, Oxford Diffraction Ltd.'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            38135
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    3.415
_exptl_absorpt_correction_T_max  0.4823
_exptl_absorpt_correction_T_min  0.3420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis RED'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.156
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       flake
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.545
_refine_diff_density_min         -0.894
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     986
_refine_ls_number_reflns         14039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0395P)^2^+15.1933P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0809
_reflns_number_gt                12437
_reflns_number_total             14039
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b823294f.txt
_cod_data_source_block           complex1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7001454