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_7014312
_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         'C35 H67 B N6 O Si2 Sm, 2(C7 H14)'
_chemical_formula_sum            'C49 H95 B N6 O Si2 Sm'
_chemical_formula_weight         1001.65
_chemical_name_systematic
;
?
;
_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
_cell_angle_alpha                65.7920(10)
_cell_angle_beta                 70.6740(10)
_cell_angle_gamma                89.696(2)
_cell_formula_units_Z            2
_cell_length_a                   12.1033(9)
_cell_length_b                   16.3329(13)
_cell_length_c                   16.7012(13)
_cell_measurement_reflns_used    5146
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.874
_cell_measurement_theta_min      2.384
_cell_volume                     2808.7(4)
_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    'DIRDIF-96 (Beurskens et al., 1996)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0588
_diffrn_reflns_av_sigmaI/netI    0.1021
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21176
_diffrn_reflns_theta_full        26.46
_diffrn_reflns_theta_max         26.46
_diffrn_reflns_theta_min         1.38
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.125
_exptl_absorpt_correction_T_max  0.9356
_exptl_absorpt_correction_T_min  0.7740
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Bruker SHELXTL (Bruker, 1997)'
_exptl_crystal_colour            green-black
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
The SQUEEZE routine (Sluis, P. van der; Spek, A. L. Acta
Crystallogr. 1990, A46, 194-201) of the program PLATON (Spek, A. L.
Acta Crystogr. 1990, A46, C-34) was used to remove the contributions
of the two disordered solvent methylcyclohexane molecules to the
observed structure factors. A large (934 cubic Angstroms) void
centred at (0.036, 0.456, 0.500) with scattering associated with a
total density equivalent to 218 electrons was found and attributed
to the four molecules of methylcyclohexane located within in the unit
cell (i.e. two solvent molecules per molecule of the Sm complex).
;
_refine_diff_density_max         1.246
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         11447
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1175
_reflns_number_gt                8354
_reflns_number_total             11447
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            C0DT00162G.TXT
_cod_data_source_block           5a-Sm
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_database_code               7014312