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_4089253
_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         'C40 H51 Cl N2 O3 Sn W'
_chemical_formula_sum            'C40 H51 Cl N2 O3 Sn W'
_chemical_formula_weight         945.82
_chemical_name_systematic        LY-661
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 93.433(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5891(15)
_cell_length_b                   18.986(3)
_cell_length_c                   19.570(3)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.21
_cell_volume                     3927.4(10)
_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 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.0253
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27861
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.996
_diffrn_reflns_theta_min         2.385
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    3.668
_exptl_absorpt_correction_T_max  0.2169
_exptl_absorpt_correction_T_min  0.2169
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.6
_refine_diff_density_max         1.934
_refine_diff_density_min         -2.032
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         9424
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0309
_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^)+12.7045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0601
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8239
_reflns_number_total             9424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00110_si_002.cif
_cod_data_source_block           greg1550f
_cod_original_cell_volume        3927.4(9)
_cod_database_code               4089253
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.217
_shelx_estimated_absorpt_t_min   0.217
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 W-Sn \\sim W-SnS
 with sigma of 0.0005
 Sn-Cl \\sim SnS-ClS
 with sigma of 0.002
 Sn-C1 \\sim SnS-C1
 with sigma of 0.002
3. Rigid bond restraints
 C5, C6, C4, 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
Sn \\sim SnS: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
Cl \\sim ClS: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
5. Others
 Sof(SnS)=Sof(ClS)=1-FVAR(1)
 Sof(Sn)=Sof(Cl)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C25(H25), C28(H28)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C9(H9), C10(H10), C11(H11), C21(H21), C22(H22), C23(H23)
6.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C),
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              56462
_shelx_hkl_checksum              94789
_olex2_submission_special_instructions 'No special instructions were received'