Sandwich Lutetacyclopentadiene with the Coordination of Lithium to the Diene Unit: Synthesis, Structure, and Transformation
Xu, Ling; Wang, Yang; Wang, Yu-Chen; Wang, Zitao; Zhang, Wen-Xiong; Xi, Zhenfeng; Organometallics 35 (2015) 5–; doi:10.1021/acs.organomet.5b00957

data_4088244
_publ_section_title
;
 Sandwich Lutetacyclopentadiene with the Coordination of Lithium to the
 Diene Unit: Synthesis, Structure, and Transformation
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              5
_journal_paper_doi               10.1021/acs.organomet.5b00957
_journal_volume                  35
_journal_year                    2015
_chemical_formula_moiety         'C44 H62 K Lu O6 Si2, C7 H8'
_chemical_formula_sum            'C51 H70 K Lu O6 Si2'
_chemical_formula_weight         1049.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-07-05
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.262(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3346(7)
_cell_length_b                   11.0051(3)
_cell_length_c                   26.0334(10)
_cell_measurement_reflns_used    8380
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      27.4670
_cell_measurement_theta_min      3.7230
_cell_volume                     5248.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.9980
_diffrn_measured_fraction_theta_max 0.8776
_diffrn_measurement_details
;
  1 omega  -20.00   29.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.3430  -99.0000    0.0000 49

  2 omega  -87.00    2.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.3430  -77.0000   30.0000 89

  3 omega  -31.00   68.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.3430   19.0000 -180.0000 99
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0169244000
_diffrn_orient_matrix_UB_12      -0.0119043000
_diffrn_orient_matrix_UB_13      0.0244688000
_diffrn_orient_matrix_UB_21      -0.0315808000
_diffrn_orient_matrix_UB_22      0.0212711000
_diffrn_orient_matrix_UB_23      0.0120175000
_diffrn_orient_matrix_UB_31      -0.0146943000
_diffrn_orient_matrix_UB_32      -0.0596516000
_diffrn_orient_matrix_UB_33      -0.0006080000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            28758
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         2.893
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.050
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       needle
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.367
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         10341
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0197P)^2^+1.9499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0680
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8021
_reflns_number_total             10341
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00957_si_002.cif
_cod_data_source_block           4
_cod_database_code               4088244
_chemical_oxdiff_formula         'C52 H43 K Lu Si2 O6'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,
 H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B),
 C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28),
  C29(H29), C30(H30), C31(H31), C32(H32), C45(H45), C46(H46), C47(H47),
 C48(H48), C49(H49)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C20(H20A,H20B,H20C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C51(H51A,H51B,H51C)
;
_shelx_estimated_absorpt_t_max   0.685
_shelx_estimated_absorpt_t_min   0.685
_shelx_hkl_checksum              81197