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_7054829
_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_moiety         'C47 H79 B N11 Sm'
_chemical_formula_sum            'C47 H79 B N11 Sm'
_chemical_formula_weight         959.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 90.3416(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9188(9)
_cell_length_b                   16.8238(11)
_cell_length_c                   21.9614(15)
_cell_measurement_reflns_used    4517
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      20.19
_cell_measurement_theta_min      2.21
_cell_volume                     5142.5(6)
_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-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.975
_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  0.0435
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            41002
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.144
_diffrn_reflns_theta_min         1.525
_exptl_absorpt_coefficient_mu    1.183
_exptl_absorpt_correction_T_max  0.9177
_exptl_absorpt_correction_T_min  0.7018
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2020
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.317
_exptl_crystal_size_min          0.185
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         12276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+1.7446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0715
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10069
_reflns_number_total             12276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj00568j2.cif
_cod_data_source_block           tak1428
_cod_depositor_comments
'Adding full bibliography for 7054827--7054829.cif.'
_cod_database_code               7054829
_shelx_estimated_absorpt_t_min   0.624
_shelx_estimated_absorpt_t_max   0.811
_shelxl_version_number           2014-3
_shelx_res_checksum              62192