Synthesis and structures of the ytterbium(ii) β-diketiminates [Yb{N(SiMe3)C(R2)C(H)C(R4)N(SiMe3)}2] (R2 = R4 = Ph, C6H4Me-4, or C6H4Ph-4; or R2 = C6H4Me-4, R4 = 1-adamantyl)
Avent, Anthony G.; Hitchcock, Peter B.; Khvostov, Alexei V.; Lappert, Michael F.; Protchenko, Andrey V.; Dalton Transactions  (2003) 1070–; doi:10.1039/b300204g

data_7012694
_publ_section_title
;
 Synthesis and structures of the ytterbium(ii)&#x00A0;\b-diketiminates
 [Yb{N(SiMe3)C(R2)C(H)C(R4)N(SiMe3)}2]&#x00A0;(R2&#x00A0;= R4&#x00A0;=
 Ph, C6H4Me-4, or C6H4Ph-4; or R2&#x00A0;= C6H4Me-4, R4&#x00A0;=
 1-adamantyl)
;
_journal_issue                   6
_journal_name_full               'Dalton Transactions'
_journal_page_first              1070
_journal_paper_doi               10.1039/b300204g
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C66 H74 N4 Si4 Yb1'
_chemical_formula_sum            'C66 H74 N4 Si4 Yb'
_chemical_formula_weight         1208.69
_chemical_name_common
;
[Yb{Me3SiNC(C6H4Ph)CHC(C6H4Ph)NSiMe3)}2]]
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/cifdics/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_date             2001-07-05T13:39:17-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1373(3)
_cell_length_b                   22.1348(5)
_cell_length_c                   23.2872(3)
_cell_measurement_reflns_used    28940
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     6256.3(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_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_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.057
_diffrn_reflns_av_unetI/netI     0.0637
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            38043
_diffrn_reflns_theta_full        27.89
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         3.81
_exptl_absorpt_coefficient_mu    1.613
_exptl_absorpt_correction_T_max  0.530
_exptl_absorpt_correction_T_min  0.508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.030(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         13613
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+3.2824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0846
_reflns_number_gt                10281
_reflns_number_total             13613
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b300204g.txt
_cod_data_source_block           jul701
_cod_original_sg_symbol_H-M      Pna2(1)
_cod_database_code               7012694