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_4089255
_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
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_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 Ge N2 O2 W, C32 H12 B F24, C4 H10 O'
_chemical_formula_sum            'C75 H73 B F24 Ge N2 O3 W'
_chemical_formula_weight         1773.60
_chemical_name_systematic        LY-804
_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                 111.7740(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.8610(3)
_cell_length_b                   18.8392(3)
_cell_length_c                   21.7896(3)
_cell_measurement_reflns_used    20591
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      1.00
_cell_volume                     7952.4(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.988
_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  0.0781
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            102498
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_min         2.309
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.925
_exptl_absorpt_correction_T_max  0.8308
_exptl_absorpt_correction_T_min  0.5131
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       block
_exptl_crystal_F_000             3552
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.825
_refine_diff_density_min         -1.395
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1053
_refine_ls_number_reflns         18966
_refine_ls_number_restraints     182
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0827P)^2^+5.3643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1411
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13866
_reflns_number_total             18966
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00110_si_002.cif
_cod_data_source_block           1978
_cod_database_code               4089255
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.831
_shelx_estimated_absorpt_t_min   0.513
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H39A,H39B,H39C} of C39, {H29A,H29B,H29C} of C29, {H26A,
  H26B,H26C} of C26, {H36A,H36B,H36C} of C36, {H37A,H37B,H37C} of C37, {H35A,
  H35B,H35C} of C35, {H28A,H28B,H28C} of C28, {H38A,H38B,H38C} of C38, {H25A,
  H25B,H25C} of C25, {H16A,H16B,H16C} of C16, {H14A,H14B,H14C} of C14, {H17A,
  H17B,H17C} of C17, {H13A,H13B,H13C} of C13, All C(H,H) groups
 At 1.5 times of:
  {H72A,H72B,H72C} of C72, {H75A,H75B,H75C} of C75
2. Restrained distances
 C74-C75
 1.5 with sigma of 0.002
3. Rigid bond restraints
 C54, F9
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F18, F16T
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C62, F14
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C63, F17
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C70, F21
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C42, C46
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C5, W
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
F17 \\sim F18 \\sim F16 \\sim F16S \\sim F16T: within 2A with sigma of 0.002
and sigma for terminal atoms of 0.004
C44 \\sim C47 \\sim F4 \\sim F5 \\sim F6: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004
Uanis(F1) \\sim Ueq, Uanis(F1S) \\sim Ueq, Uanis(F2S) \\sim Ueq, Uanis(F3)
\\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F7S) \\sim Ueq, Uanis(F9) \\sim Ueq,
Uanis(F13) \\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F16S) \\sim Ueq, Uanis(F16T)
\\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F13S) \\sim Ueq, Uanis(F14S) \\sim Ueq,
Uanis(F15S) \\sim Ueq, Uanis(F21) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(C13) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C75)
\\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
5. Others
 Sof(F13S)=1-FVAR(1)
 Sof(F13)=FVAR(1)
 Sof(F1S)=Sof(F2S)=Sof(F14S)=Sof(F15S)=1-FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F14)=Sof(F15)=FVAR(2)
 Fixed Sof: F7(0.3) F7S(0.7) F16(0.6) F16S(0.2) F16T(0.2)
6.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27)
6.b Secondary CH2 refined with riding coordinates:
 C73(H73A,H73B), C74(H74A,H74B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22),
 C41(H41), C43(H43), C45(H45), C49(H49), C51(H51), C53(H53), C57(H57), C59(H59),
  C61(H61), C65(H65), C67(H67), C69(H69)
6.d 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), C26(H26A,H26B,H26C), 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), C72(H72A,H72B,H72C), C75(H75A,H75B,
 H75C)
;
_shelx_res_checksum              71867
_shelx_hkl_checksum              33641
_olex2_submission_special_instructions 'No special instructions were received'