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_4341397
_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, 2(C6 H6), I'
_chemical_formula_sum            'C66 H104 B2 I N12 Tm'
_chemical_formula_weight         1383.06
_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                 94.9815(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.3130(6)
_cell_length_b                   20.6488(6)
_cell_length_c                   17.1556(5)
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.34
_cell_volume                     6815.6(4)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            59085
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.06
_exptl_absorpt_coefficient_mu    1.802
_exptl_absorpt_correction_T_max  0.7316
_exptl_absorpt_correction_T_min  0.4873
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         15664
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0221
_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^)+(0.0183P)^2^+5.1100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0476
_refine_ls_wR_factor_ref         0.0533
_reflns_number_gt                13433
_reflns_number_total             15664
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic501816v_si_002.cif
_cod_data_source_block           3TmPlus
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4341397
_shelxl_version_number           2008-4
_shelx_res_checksum              25363
_shelx_hkl_checksum              72390