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_4341398
_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         'C42 H68 B2 N12 Tm, C4 H10 O2'
_chemical_formula_sum            'C46 H78 B2 N12 O2 Tm'
_chemical_formula_weight         1021.75
_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                 104.336(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.3322(17)
_cell_length_b                   21.988(3)
_cell_length_c                   11.0351(17)
_cell_measurement_reflns_used    5285
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19.96
_cell_measurement_theta_min      2.31
_cell_volume                     2664.0(7)
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0680
_diffrn_reflns_av_sigmaI/netI    0.0552
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            21332
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    1.711
_exptl_absorpt_correction_T_max  0.8925
_exptl_absorpt_correction_T_min  0.5763
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1066
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
Attempts to refine peaks of residual electron density as disordered or 
partial-occupancy solvent dimethoxyethane oxygen or carbon atoms were 
unsuccessful.  The data were corrected for disordered electron density 
through use of the SQUEEZE procedure (Sluis, P. van der; Spek, A. L. Acta 
Crystallogr. 1990, A46, 194&#x0096;201) as implemented in PLATON (Spek, A. L. 
Acta Crystallogr. 1990, A46, C34; Spek, A. L. J. Appl. Cryst. 2003, 36, 
7&#x0096;13.  PLATON - a multipurpose crystallographic tool.  Utrecht University, 
Utrecht, The Netherlands).  A total solvent-accessible void volume of 
542 &#x00C5;3 with a total electron count of 110 (consistent with 2 molecules 
of solvent dimethoxyethane, or 1 molecule per formula unit of the 
[{HB(3,5-Me2-4-Et-pyrazolyl)3}2Tm] molecule) was found in the unit cell.;
;
_refine_diff_density_max         1.532
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         5496
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+15.5339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1484
_reflns_number_gt                3731
_reflns_number_total             5496
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic501816v_si_002.cif
_cod_data_source_block           4Tm
_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               4341398
_shelxl_version_number           2008-4
_shelx_res_checksum              17055
_shelx_hkl_checksum              17411