Reactions of lanthanoid metals with 3,5-diphenylpyrazole at elevated temperatures: synthesis and structures of both homoleptic, [Ln3(Ph2pz)9] (Ln = La, Nd), [Ln2(Ph2pz)6] (Ln = Er, Lu), and heteroleptic, [Ln(Ph2pz)3(Ph2pzH)2] (Ln = La, Nd, Gd, Tb, Er or Yb), pyrazolate complexes.
Deacon, Glen B.; Forsyth, Craig M.; Gitlits, Alex; Skelton, Brian W.; White, Allan H.; Dalton transactions (Cambridge, England : 2003)  (2004) 1239–1247; doi:10.1039/b400541d

data_7014052
_publ_section_title
;
 Reactions of lanthanoid metals with 3,5-diphenylpyrazole at elevated
 temperatures: synthesis and structures of both homoleptic,
 [Ln3(Ph2pz)9] (Ln = La, Nd), [Ln2(Ph2pz)6] (Ln = Er, Lu), and
 heteroleptic, [Ln(Ph2pz)3(Ph2pzH)2] (Ln = La, Nd, Gd, Tb, Er or Yb),
 pyrazolate complexes.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1239
_journal_page_last               1247
_journal_paper_doi               10.1039/b400541d
_journal_year                    2004
_chemical_formula_sum            'C90 H66 Lu2 N12'
_chemical_formula_weight         1665.5
_chemical_name_systematic
;
Hexakis(3,5-diphenylpyrazolato)dilutetium(III)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.180(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7838(2)
_cell_length_b                   18.9626(4)
_cell_length_c                   30.0967(5)
_cell_measurement_reflns_used    N/A
_cell_measurement_temperature    123(2)
_cell_volume                     7221.6(2)
_computing_cell_refinement       'DENZO-SMN (Otwinoski and Minor, 1993)'
_computing_data_collection       'COLLECT (Nonius BV, 1994)'
_computing_data_reduction        'DENZO-SMN (Otwinoski and Minor, 1993)'
_computing_molecular_graphics    'SHELXTL-PLUS (Siemans, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type
;
Enraf Nonius CCD
;
_diffrn_measurement_method       'phi 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  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            64198
_diffrn_reflns_theta_full        27.84
_diffrn_reflns_theta_max         27.84
_diffrn_reflns_theta_min         1.27
_diffrn_standards_number         N/A?
_exptl_absorpt_coefficient_mu    2.776
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3328
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.272
_refine_diff_density_min         -2.926
_refine_diff_density_rms         0.472
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     937
_refine_ls_number_reflns         16054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0897P)^2^+17.0682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1654
_reflns_number_gt                12620
_reflns_number_total             16054
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b400541d.txt
_cod_data_source_block           lupza
_cod_original_cell_volume        7222(3)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7014052
_exptl_absorpt_correction_a_min  0.73
_exptl_absorpt_correction_a_max  0.76