Investigation of the “bent sandwich-like” divalent lanthanide hydro-tris(pyrazolyl)borates Ln(TpiPr2)2(Ln = Sm, Eu, Tm, Yb)
Kühling, Marcel; Wickleder, Claudia; Ferguson, Michael J.; Hrib, Cristian G.; McDonald, Robert; Suta, Markus; Hilfert, Liane; Takats, Josef; Edelmann, Frank T.; New J. Chem. 39 (2015) 7617–; doi:10.1039/C5NJ00568J

data_7054827
_publ_section_title
;
 Investigation of the &#x201C;bent sandwich-like&#x201D; divalent
 lanthanide hydro-tris(pyrazolyl)borates Ln(TpiPr2)2(Ln = Sm, Eu, Tm, Yb)
;
_journal_issue                   10
_journal_name_full               'New J. Chem.'
_journal_page_first              7617
_journal_paper_doi               10.1039/C5NJ00568J
_journal_volume                  39
_journal_year                    2015
_chemical_formula_sum            'C59 H104 B2 N12 Yb'
_chemical_formula_weight         1176.20
_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
_audit_update_record
;
2015-02-26 deposited with the CCDC.
2015-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                83.2050(10)
_cell_angle_beta                 74.7430(10)
_cell_angle_gamma                77.6100(10)
_cell_formula_units_Z            4
_cell_length_a                   13.44670(10)
_cell_length_b                   20.6731(2)
_cell_length_c                   25.1841(2)
_cell_measurement_reflns_used    79913
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.1670
_cell_measurement_theta_min      2.4150
_cell_volume                     6582.53(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            488976
_diffrn_reflns_theta_full        30.91
_diffrn_reflns_theta_max         30.91
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    1.464
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.989
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1345
_refine_ls_number_reflns         39188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0202P)^2^+7.8777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0689
_reflns_number_gt                32776
_reflns_number_total             39188
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj00568j2.cif
_cod_data_source_block           magd113
_cod_depositor_comments
'Adding full bibliography for 7054827--7054829.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7054827