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_7054828
_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            'C56 H95 B2 N13 Sm'
_chemical_formula_weight         1122.41
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-02-26 deposited with the CCDC.
2015-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                104.2666(8)
_cell_angle_beta                 94.8690(8)
_cell_angle_gamma                115.6405(7)
_cell_formula_units_Z            2
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_cell_length_b                   13.6332(10)
_cell_length_c                   20.9744(16)
_cell_measurement_reflns_used    9807
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.16
_cell_volume                     3167.5(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            27037
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.575
_diffrn_reflns_theta_min         1.027
_exptl_absorpt_coefficient_mu    0.971
_exptl_absorpt_correction_T_max  0.9011
_exptl_absorpt_correction_T_min  0.7450
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS 2014/2 (Sheldrick 2008)'
_exptl_crystal_colour            green
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_exptl_crystal_description       block
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_exptl_crystal_size_max          0.515
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_exptl_crystal_size_min          0.194
_refine_diff_density_max         0.788
_refine_diff_density_min         -1.115
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         14330
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+1.2456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12864
_reflns_number_total             14330
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj00568j2.cif
_cod_data_source_block           tak1426
_cod_depositor_comments
'Adding full bibliography for 7054827--7054829.cif.'
_cod_database_code               7054828
_shelx_estimated_absorpt_t_min   0.635
_shelx_estimated_absorpt_t_max   0.834
_shelxl_version_number           2014-3
_shelx_res_checksum              44950