Unusual reactivity of lanthanide borohydride complexes leading to a borane complex
Meyer, Nils; Jenter, Jelena; Roesky, Peter W.; Eickerling, Georg; Scherer, Wolfgang; Chemical Communications  (2009) 4693–4695; doi:10.1039/b907193h

data_7111543
_publ_section_title
;
 Unusual reactivity of lanthanide borohydride complexes leading to a
 borane complex
;
_journal_issue                   31
_journal_name_full               'Chemical Communications'
_journal_page_first              4693
_journal_page_last               4695
_journal_paper_doi               10.1039/b907193h
_journal_year                    2009
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C38 H62 B2 Lu N3 O2, 2(C4 H8 O)'
_chemical_formula_sum            'C46 H78 B2 Lu N3 O4'
_chemical_formula_weight         933.70
_chemical_name_systematic        ?
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      7
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 100.420(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5587(9)
_cell_length_b                   15.1757(17)
_cell_length_c                   16.1030(19)
_cell_measurement_reflns_used    10940
_cell_measurement_temperature    6(2)
_cell_measurement_theta_max      30.42
_cell_measurement_theta_min      3.03
_cell_volume                     2297.4(4)
_computing_cell_refinement       'EVAL14 (Duisenberg, 2003)'
_computing_data_collection       'FD345 (Weber, 2004)'
_computing_data_reduction        'EVAL14 (Duisenberg, 2003)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      6(2)
_diffrn_detector                 'image plate'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'MAR345 MARRESEARCH'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.779
_diffrn_measurement_device_type  '4 circle euler goniometer HUBER'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'rotating Anode FR591 BRUKER'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13834
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         30.23
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    2.192
_exptl_absorpt_correction_T_max  0.814
_exptl_absorpt_correction_T_min  0.688
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.091
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.016(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         8265
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0)^2^+6.1344P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0618
_reflns_number_gt                8047
_reflns_number_total             8265
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b907193hsup1.cif
_cod_data_source_block           roesky
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               7111543