Polynuclear lanthanide (Ln) complexes of a tri-functional hydrazone ligand‒mononuclear (Dy), dinuclear (Yb, Tm), tetranuclear (Gd), and hexanuclear (Gd, Dy, Tb) examples.
Anwar, Muhammad U.; Dawe, Louise N.; Tandon, Santokh S.; Bunge, Scott D.; Thompson, Laurence K.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 7781–7794; doi:10.1039/c3dt32732a

data_7022665
_publ_section_title
;
 Polynuclear lanthanide (Ln) complexes of a tri-functional hydrazone
 ligand--mononuclear (Dy), dinuclear (Yb, Tm), tetranuclear (Gd), and
 hexanuclear (Gd, Dy, Tb) examples.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7781
_journal_page_last               7794
_journal_paper_doi               10.1039/c3dt32732a
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C84 H100 Gd6 N19 O45'
_chemical_formula_sum            'C84 H100 Gd6 N19 O45'
_chemical_formula_weight         3039.31
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                80.002(6)
_cell_angle_beta                 68.785(5)
_cell_angle_gamma                75.752(5)
_cell_formula_units_Z            2
_cell_length_a                   17.8448(13)
_cell_length_b                   18.4743(14)
_cell_length_c                   20.2807(15)
_cell_measurement_reflns_used    39802
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     6014.6(8)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL-97: Acta Cryst.2008, A64, 112-122'
_computing_structure_solution    'SHELXS-97: Acta Cryst.2008, A64, 112-122'
_diffrn_ambient_temperature      163(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'graphite - Rigaku SHINE'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0694
_diffrn_reflns_av_sigmaI/netI    0.1077
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            51765
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    3.347
_exptl_absorpt_correction_T_max  0.668
_exptl_absorpt_correction_T_min  0.413
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2962
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
The Platon SQUEEZE procedure was applied to recover 270 electrons per
unit cell in three voids that were sufficiently large to contain a small
molecule (total volume 1153 ^A^3); that is 135 electrons
per formula unit. Void 1 and 2 are considered to each contain a water
molecule (10 electrons; one water molecule per formula unit), while
void 4 is sufficiently large, and contains enough electrons, to account
for the missing 0.5 protonated triethylamine (51 electrons), as well as
six additional water molecules. These have been included in the formula
for the calculation of intensive properties.
PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13.
;
_refine_diff_density_max         12.756
_refine_diff_density_min         -2.631
_refine_diff_density_rms         0.333
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1341
_refine_ls_number_reflns         24712
_refine_ls_number_restraints     182
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0925
_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^)+(0.1358P)^2^+122.7354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2478
_refine_ls_wR_factor_ref         0.2571
_reflns_number_gt                20749
_reflns_number_total             24712
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt32732a.txt
_cod_data_source_block           1_Revised
_cod_database_code               7022665