Syntheses and Structures of the Crystalline, Highly Crowded 1,3-Bis(trimethylsilyl)cyclopentadienyls [MCp″3] (M = Y, Er, Yb), [PbCp″2], [{YCp″2(μ-OH)}2], [(ScCp″2)2(μ-η2:η2-C2H4)], [YbCp″2Cl(μ-Cl)K(18-crown-6)], and [{KCp″}∞]
Coles, Martyn P.; Hitchcock, Peter B.; Lappert, Michael F.; Protchenko, Andrey V.; Organometallics 31 (2012) 2682–; doi:10.1021/om2009364

data_4077884
_publ_section_title
;
 Syntheses and Structures of the Crystalline, Highly Crowded
 1,3-Bis(trimethylsilyl)cyclopentadienyls [MCp&#x2033;3] (M = Y, Er, Yb),
 [PbCp&#x2033;2], [{YCp&#x2033;2(\m-OH)}2],
 [(ScCp&#x2033;2)2(\m-\h2:\h2-C2H4)],
 [YbCp&#x2033;2Cl(\m-Cl)K(18-crown-6)], and [{KCp&#x2033;}\\infty ]
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2682
_journal_paper_doi               10.1021/om2009364
_journal_volume                  31
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C33 H63 Si6 Y1'
_chemical_formula_structural     'C33 H63 SI6 Y'
_chemical_formula_sum            'C33 H63 Si6 Y'
_chemical_formula_weight         717.28
_chemical_name_common            '[Y{C5H3(SiMe3)2}3]'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location
ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_creation_date             1999-12-14T10:36:17-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 112.724(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6641(5)
_cell_length_b                   13.6340(4)
_cell_length_c                   19.1235(5)
_cell_measurement_reflns_used    14214
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      4.246
_cell_measurement_wavelength     0.71073
_cell_volume                     4248.1(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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0792
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29506
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         4.25
_exptl_absorpt_coefficient_mu    1.561
_exptl_absorpt_correction_T_max  0.7212
_exptl_absorpt_correction_T_min  0.665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         12277
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0192P)^2^+4.3252P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.089
_refine_ls_wR_factor_ref         0.1029
_reflns_number_gt                8337
_reflns_number_total             12277
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2009364_si_001.cif
_cod_data_source_block           (1Y)-dec1499
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4077884