Heteroleptic ytterbium(ii) complexes supported by a bulky β-diketiminato ligand
Hitchcock, Peter B.; Khvostov, Alexei V.; Lappert, Michael F.; Protchenko, Andrey V.; Dalton Transactions  (2009) 2383–2391; doi:10.1039/b818969b

data_7000841
_publ_section_title
;
 Heteroleptic ytterbium(ii) complexes supported by a bulky
 \b-diketiminato ligand
;
_journal_issue                   13
_journal_name_full               'Dalton Transactions'
_journal_page_first              2383
_journal_page_last               2391
_journal_paper_doi               10.1039/b818969b
_journal_year                    2009
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C46 H46 O2 Yb, C7 H8'
_chemical_formula_sum            'C53 H54 O2 Yb'
_chemical_formula_weight         896
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2004-05-13T11:47:01-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                111.214(1)
_cell_angle_beta                 96.485(1)
_cell_angle_gamma                91.056(1)
_cell_formula_units_Z            4
_cell_length_a                   10.1293(2)
_cell_length_b                   20.7321(4)
_cell_length_c                   21.6554(5)
_cell_measurement_reflns_used    92121
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.682
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     4203.73(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.262183E-1
_diffrn_orient_matrix_UB_12      0.392123E-1
_diffrn_orient_matrix_UB_13      -0.143447E-1
_diffrn_orient_matrix_UB_21      0.904339E-1
_diffrn_orient_matrix_UB_22      0.29304E-2
_diffrn_orient_matrix_UB_23      -0.135236E-1
_diffrn_orient_matrix_UB_31      -0.323606E-1
_diffrn_orient_matrix_UB_32      -0.337919E-1
_diffrn_orient_matrix_UB_33      -0.458922E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            63001
_diffrn_reflns_theta_full        25.7
_diffrn_reflns_theta_max         25.7
_diffrn_reflns_theta_min         3.72
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    2.265
_exptl_absorpt_correction_T_max  0.7668
_exptl_absorpt_correction_T_min  0.6447
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.11
_refine_diff_density_min         -1.741
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     952
_refine_ls_number_reflns         15191
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+27.7120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1334
_refine_ls_wR_factor_ref         0.1409
_reflns_number_gt                12460
_reflns_number_total             15191
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b818969b.txt
_cod_data_source_block           (9)-may804
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7000841