Binuclear rare-earth polyhydride complexes bearing both terminal and bridging hydride ligands
Cheng, Jianhua; Wang, Haiyu; Nishiura, Masayoshi; Hou, Zhaomin; Chemical Science 3 (2012) 2230–; doi:10.1039/c2sc20300f

data_1515050
_publ_section_title
;
 Binuclear rare-earth polyhydride complexes bearing both terminal and
 bridging hydride ligands
;
_journal_issue                   7
_journal_name_full               'Chemical Science'
_journal_page_first              2230
_journal_paper_doi               10.1039/c2sc20300f
_journal_volume                  3
_journal_year                    2012
_chemical_formula_sum            'C81 H114 Lu2 N4 O3'
_chemical_formula_weight         1541.70
_chemical_name_common            ((Ph-NCN)LuH2)2(THF)3
_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                81.780(2)
_cell_angle_beta                 73.628(2)
_cell_angle_gamma                66.103(2)
_cell_formula_units_Z            2
_cell_length_a                   13.2117(18)
_cell_length_b                   14.827(2)
_cell_length_c                   23.057(3)
_cell_measurement_temperature    163(2)
_cell_volume                     3959.9(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'CCD area detector'
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21538
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    2.524
_exptl_absorpt_correction_T_max  0.7033
_exptl_absorpt_correction_T_min  0.4720
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1588
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
1/2 disorder Et2O molecule per formual unit of [(Ph-NCN)LuH2]2(THF)3
was not modelled and the disordered density was taken into account
using the SQUEEZE/PLATON procedure.(Sluis, P. van der;
Spek, A. L. Acta Crystallogr. 1990, A46, 194?01) as implemented in
PLATON (Spek, A.L. Acta Crystallogr. 1990, A46, C34; Spek,
A.L. J. Appl. Cryst. 2003, 36, 7?3. PLATON - a multipurpose
crystallographic tool. Utrecht University, Utrecht, The Netherlands).
;
_refine_diff_density_max         3.566
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     798
_refine_ls_number_reflns         13729
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0713P)^2^+5.5405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1317
_reflns_number_gt                11107
_reflns_number_total             13729
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2sc20300f.txt
_cod_data_source_block           1-Lu
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/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 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        3960.1(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1515050