To Bend or Not To Bend: Experimental and Computational Studies of Structural Preference in Ln(Tp(iPr)2)2 (Ln = Sm, Tm).
Momin, Aurélien; Carter, Lee; Yang, Yi; McDonald, Robert; Essafi Née Labouille, Stéphanie; Nief, François; Del Rosal, Iker; Sella, Andrea; Maron, Laurent; Takats, Josef; Inorganic chemistry  (2014) 141027132008003–; doi:10.1021/ic501816v

data_4341396
_publ_section_title
;
 To Bend or Not To Bend: Experimental and Computational Studies of
 Structural Preference in Ln(Tp(iPr)2)2 (Ln = Sm, Tm).
;
_journal_name_full               'Inorganic chemistry'
_journal_page_first              141027132008003
_journal_paper_doi               10.1021/ic501816v
_journal_year                    2014
_chemical_formula_moiety         'C54 H92 B2 N12 Tm, 1.25(C5 H12)'
_chemical_formula_sum            'C60.25 H107 B2 N12 Tm'
_chemical_formula_weight         1190.13
_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                90.2240(6)
_cell_angle_beta                 105.4347(6)
_cell_angle_gamma                102.2972(6)
_cell_formula_units_Z            4
_cell_length_a                   13.5026(7)
_cell_length_b                   20.7331(10)
_cell_length_c                   25.3589(12)
_cell_measurement_reflns_used    9387
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.88
_cell_measurement_theta_min      2.28
_cell_volume                     6672.3(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-97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF-2008 (Beurskens et al., 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            54291
_diffrn_reflns_theta_full        26.53
_diffrn_reflns_theta_max         26.53
_diffrn_reflns_theta_min         0.83
_exptl_absorpt_coefficient_mu    1.373
_exptl_absorpt_correction_T_max  0.6623
_exptl_absorpt_correction_T_min  0.5975
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2526
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.989
_refine_diff_density_min         -1.603
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1347
_refine_ls_number_reflns         27562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+3.4603P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0918
_reflns_number_gt                23805
_reflns_number_total             27562
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic501816v_si_002.cif
_cod_data_source_block           3Tm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 
;
_cod_database_code               4341396
_shelxl_version_number           2008-4
_shelx_res_checksum              48088
_shelx_hkl_checksum              11879