Stable heteroleptic complexes of divalent lanthanides with bulky pyrazolylborate ligands‒iodides, hydrocarbyls and triethylborohydrides.
Zhang, X. W.; Maunder, Graham H.; Giessmann, Stefan; MacDonald, Robert; Ferguson, Michael J.; Bond, Andrew H.; Rogers, Robin D.; Sella, Andrea; Takats, Josef; Dalton transactions (Cambridge, England : 2003) 40 (2011) 195–210; doi:10.1039/c0dt00162g

data_7014313
_publ_section_title
;
 Stable heteroleptic complexes of divalent lanthanides with bulky
 pyrazolylborate ligands--iodides, hydrocarbyls and
 triethylborohydrides.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              195
_journal_page_last               210
_journal_paper_doi               10.1039/c0dt00162g
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C31 H59 B N6 Si2 Sm, 1.5(C7 H8)'
_chemical_formula_sum            'C41.5 H71 B N6 Si2 Sm'
_chemical_formula_weight         871.38
_chemical_name_systematic
;
?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 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                 106.6876(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.8391(18)
_cell_length_b                   11.9006(12)
_cell_length_c                   24.176(3)
_cell_measurement_reflns_used    4300
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.85
_cell_measurement_theta_min      2.45
_cell_volume                     4916.3(9)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w 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  0.0647
_diffrn_reflns_av_sigmaI/netI    0.0682
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            32605
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.26
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.275
_exptl_absorpt_correction_T_max  0.8417
_exptl_absorpt_correction_T_min  0.5626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1828
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;
Attempts to refine peaks of residual electron density as
carbon atoms of a second full-occupancy molecule of solvent toluene
were unsuccessful. The data were corrected for disordered electron
density through use of the SQUEEZE procedure (Sluis, P. van der; Spek,
A. L. Acta Crystallogr. 1990, A46, 194-201) as implemented in PLATON
(Spek, A.L. Acta Crystallogr. 1990, A46, C34. PLATON - a multipurpose
crystallographic tool. Utrecht University, Utrecht, The Netherlands).
A total solvent-accessible void volume of 983.5 cubic Angstroms with a
total electron count of 271 (consistent with four molecules of solvent
toluene, or one molecule per formula unit of the samarium complex) was
found in the unit cell.
;
_refine_diff_density_max         0.976
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         10069
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0678P)^2^+0.9449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1347
_reflns_number_gt                7249
_reflns_number_total             10069
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            C0DT00162G.TXT
_cod_data_source_block           5-Sm
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_cell_volume        4916.4(9)
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_original_formula_sum        'C41.50 H71 B N6 Si2 Sm'
_cod_database_code               7014313