Synthesis and structure of divalent thulium borohydrides, and their application in 'epsilon'-caprolactone polymerisation
Aurelien Momin; Fanny Bonnet; Marc Visseaux; Laurent Maron; Josef Takats; Michael J. Ferguson; Xavier-Frederic Le Goff; Francois Nief; Chem.Commun. 47 (2011) 12203–12205; doi:10.1039/c1cc15294g

data_7107021
_publ_section_title
;
 Synthesis and structure of divalent thulium borohydrides, and their
 application in 'epsilon'-caprolactone polymerisation
;
_journal_issue                   44
_journal_name_full               Chem.Commun.
_journal_page_first              12203
_journal_page_last               12205
_journal_paper_doi               10.1039/c1cc15294g
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C8 H28 B2 O4 Tm'
_chemical_formula_sum            'C8 H28 B2 O4 Tm'
_chemical_formula_weight         378.85
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 102.472(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.734(1)
_cell_length_b                   12.631(1)
_cell_length_c                   14.616(1)
_cell_measurement_reflns_used    3401
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     1574.4(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Kappa APEXII CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9931
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    5.628
_exptl_absorpt_correction_T_max  0.3990
_exptl_absorpt_correction_T_min  0.3017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor, 1996)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.081
_refine_diff_density_min         -0.861
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       0.0004(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         4549
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0276
_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^)+(0.0000P)^2^+5.0314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0628
_reflns_number_gt                4128
_reflns_number_total             4549
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc15294g.txt
_cod_data_source_block           amx530
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P21/c '
_cod_database_code               7107021