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_4088245
_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         'C32 H38 Lu Si2, C18 H36 K N2 O6'
_chemical_formula_sum            'C50 H74 K Lu N2 O6 Si2'
_chemical_formula_weight         1069.36
_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             2015-04-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.299(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1023(2)
_cell_length_b                   18.3997(5)
_cell_length_c                   25.5155(7)
_cell_measurement_reflns_used    11110
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      27.9530
_cell_measurement_theta_min      3.3050
_cell_volume                     5197.6(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -99.00  -74.00   1.0000    7.8500
omega____ theta____ kappa____ phi______ frames
    -      -11.6392  178.0000    0.0000 25

  2 omega  -20.00   19.00   1.0000    7.8500
omega____ theta____ kappa____ phi______ frames
    -      -11.6392  -99.0000  150.0000 39

  3 omega  -14.00   14.00   1.0000    7.8500
omega____ theta____ kappa____ phi______ frames
    -      -11.6392   82.0000  144.0000 28

  4 omega -100.00  -75.00   1.0000    7.8500
omega____ theta____ kappa____ phi______ frames
    -      -11.6392  178.0000   90.0000 25

  5 omega  -12.00   52.00   1.0000    7.8500
omega____ theta____ kappa____ phi______ frames
    -      -11.6392   38.0000   30.0000 64

  6 omega  -67.00   11.00   1.0000    7.8500
omega____ theta____ kappa____ phi______ frames
    -      -11.6392  -77.0000  -90.0000 78
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0358304000
_diffrn_orient_matrix_UB_12      0.0038274000
_diffrn_orient_matrix_UB_13      0.0240400000
_diffrn_orient_matrix_UB_21      -0.0296363000
_diffrn_orient_matrix_UB_22      0.0332180000
_diffrn_orient_matrix_UB_23      0.0048988000
_diffrn_orient_matrix_UB_31      -0.0440684000
_diffrn_orient_matrix_UB_32      -0.0192186000
_diffrn_orient_matrix_UB_33      0.0132138000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_unetI/netI     0.0720
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            29444
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_min         2.879
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.072
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       prism
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.188
_refine_diff_density_min         -0.933
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     805
_refine_ls_number_reflns         10215
_refine_ls_number_restraints     379
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+4.0681P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0925
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7953
_reflns_number_total             10215
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00957_si_002.cif
_cod_data_source_block           5
_cod_database_code               4088245
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C67 H74 O6 N2 Lu Si2 K'
_shelx_estimated_absorpt_t_max   0.682
_shelx_estimated_absorpt_t_min   0.491
_reflns_odcompleteness_completeness 99.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_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. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C31) \\sim Ueq, Uanis(C31A) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(C24A)=Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27A)=
 Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=1-FVAR(1)
 Sof(C24)=Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27)=Sof(C28)=
 Sof(H28)=Sof(C29)=Sof(H29)=FVAR(1)
 Sof(Si2A)=Sof(C30A)=Sof(H30E)=Sof(H30D)=Sof(H30F)=Sof(C31A)=Sof(H31F)=
 Sof(H31D)=Sof(H31E)=Sof(C32A)=Sof(H32D)=Sof(H32F)=Sof(H32E)=1-FVAR(2)
 Sof(Si2)=Sof(C30)=Sof(H30B)=Sof(H30A)=Sof(H30C)=Sof(C31)=Sof(H31A)=Sof(H31B)=
 Sof(H31C)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(2)
 Sof(O3A)=Sof(O4A)=Sof(C39A)=Sof(H39D)=Sof(H39C)=Sof(C40A)=Sof(H40D)=Sof(H40C)=
 Sof(C41A)=Sof(H41C)=Sof(H41D)=Sof(C42A)=Sof(H42C)=Sof(H42D)=Sof(C43A)=
 Sof(H43C)=Sof(H43D)=Sof(C44A)=Sof(H44C)=Sof(H44D)=Sof(O5A)=Sof(O6A)=Sof(C45A)=
 Sof(H45C)=Sof(H45D)=Sof(C46A)=Sof(H46C)=Sof(H46D)=Sof(C47A)=Sof(H47C)=
 Sof(H47D)=Sof(C48A)=Sof(H48D)=Sof(H48C)=Sof(C49A)=Sof(H49C)=Sof(H49D)=
 Sof(C50A)=Sof(H50D)=Sof(H50C)=1-FVAR(3)
 Sof(O5)=Sof(O6)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=
 Sof(C47)=Sof(H47B)=Sof(H47A)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C49)=Sof(H49B)=
 Sof(H49A)=Sof(C50)=Sof(H50B)=Sof(H50A)=Sof(O3)=Sof(O4)=Sof(C39)=Sof(H39A)=
 Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C42)=
 Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43B)=Sof(H43A)=Sof(C44)=Sof(H44B)=Sof(H44A)=
 FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C33(H33B,H33A), C34(H34B,H34A), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,
 H37B), C38(H38A,H38B), C39A(H39D,H39C), C40A(H40D,H40C), C41A(H41C,H41D),
 C42A(H42C,H42D), C43A(H43C,H43D), C44A(H44C,H44D), C45(H45A,H45B), C46(H46A,
 H46B), C47(H47B,H47A), C48(H48A,H48B), C49(H49B,H49A), C50(H50B,H50A),
 C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43B,H43A),
  C44(H44B,H44A), C45A(H45C,H45D), C46A(H46C,H46D), C47A(H47C,H47D), C48A(H48D,
 H48C), C49A(H49C,H49D), C50A(H50D,H50C)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23),
 C25A(H25A), C26A(H26A), C27A(H27A), C28A(H28A), C29A(H29A), C25(H25), C26(H26),
  C27(H27), C28(H28), C29(H29)
5.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17C,H17A,H17B), C30A(H30E,H30D,
 H30F), C31A(H31F,H31D,H31E), C32A(H32D,H32F,H32E), C30(H30B,H30A,H30C),
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
;
_olex2_submission_special_instructions 'No special instructions were received'