Coordination Chemistry of [E(Idipp)]2+ Ligands (E = Ge, Sn): Metal Germylidyne [Cp*(CO)2W≡Ge(Idipp)]+ and Metallotetrylene [Cp*(CO)3W‒E(Idipp)]+ Cations
Lebedev, Yury N.; Das, Ujjal; Schnakenburg, Gregor; Filippou, Alexander C.; Organometallics 36 (2017) 1530–; doi:10.1021/acs.organomet.7b00110

data_4089254
_publ_section_title
;
 Coordination Chemistry of [E(Idipp)]2+ Ligands (E = Ge, Sn): Metal
 Germylidyne [Cp*(CO)2W\\tb Ge(Idipp)]+ and Metallotetrylene
 [Cp*(CO)3W--E(Idipp)]+ Cations
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1530
_journal_paper_doi               10.1021/acs.organomet.7b00110
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C39 H51 Cl Ge N2 O2 W, 0.25(C4 H10 O)'
_chemical_formula_sum            'C40 H53.5 Cl Ge N2 O2.25 W'
_chemical_formula_weight         890.23
_chemical_name_systematic        LY-703
_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
_audit_creation_date             2017-03-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                90
_cell_angle_beta                 118.8270(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8687(2)
_cell_length_b                   25.9736(5)
_cell_length_c                   16.0387(2)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      0.41
_cell_volume                     3966.64(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'fine slicing \w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_av_unetI/netI     0.0825
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41735
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         2.652
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    3.758
_exptl_absorpt_correction_T_max  0.8642
_exptl_absorpt_correction_T_min  0.7050
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'clear reddish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       plate
_exptl_crystal_F_000             1794
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.739
_refine_diff_density_min         -1.461
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         9485
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      0.930
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0413P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0912
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5991
_reflns_number_total             9485
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00110_si_002.cif
_cod_data_source_block           greg1767
_cod_original_formula_sum        'C40 H53.50 Cl Ge N2 O2.25 W'
_cod_database_code               4089254
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.864
_shelx_estimated_absorpt_t_min   0.705
_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. Restrained distances
 C40-C41 = C42-C43
 1.54 with sigma of 0.002
 C41-O3 = O3-C42
 1.48 with sigma of 0.002
 C40-O3 = O3-C43 = C41-C42
 2.54 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
C40 \\sim C41 \\sim O3 \\sim C42 \\sim C43: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004
Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43)
\\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of 0.002 and sigma for terminal
atoms of 0.004
4. Others
 Fixed Sof: O3(0.25) C40(0.25) H40A(0.25) H40B(0.25) H40C(0.25) C41(0.25)
 H41A(0.25) H41B(0.25) C42(0.25) H42A(0.25) H42B(0.25) C43(0.25) H43A(0.25)
 H43B(0.25) H43C(0.25)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27)
5.b Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C42(H42A,H42B)
5.c Me refined with riding coordinates:
 C26(H26A,H26B,H26C), C40(H40A,H40B,H40C), C43(H43A,H43B,H43C)
5.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22)
5.e Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C),
 C39(H39A,H39B,H39C)
;
_shelx_res_checksum              93851
_shelx_hkl_checksum              19410
_olex2_submission_special_instructions 'No special instructions were received'