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_4089256
_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 N2 O3 Sn W, Al C16 F36 O4, 0.5(C6 H6)'
_chemical_formula_sum            'C59 H54 Al F36 N2 O7 Sn W'
_chemical_formula_weight         1916.56
_chemical_name_systematic        LY-371
_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             2017-03-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.0240(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6260(4)
_cell_length_b                   21.2391(6)
_cell_length_c                   18.8550(3)
_cell_measurement_reflns_used    16878
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      1.00
_cell_volume                     7236.7(3)
_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
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_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  0.0552
_diffrn_reflns_av_unetI/netI     0.0704
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            55484
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         2.758
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.088
_exptl_absorpt_correction_T_max  0.8508
_exptl_absorpt_correction_T_min  0.3672
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_description       plate
_exptl_crystal_F_000             3756
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.085
_refine_diff_density_min         -1.484
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1119
_refine_ls_number_reflns         15727
_refine_ls_number_restraints     175
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0659P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1157
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11273
_reflns_number_total             15727
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00110_si_002.cif
_cod_data_source_block           greg1585
_cod_database_code               4089256
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.851
_shelx_estimated_absorpt_t_min   0.367
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H) groups
2. Rigid bond restraints
 F9, C44
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 W, C5, C6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F25, C52
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F33, C54
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C41, C43
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
F31 \\sim F32 \\sim F33 \\sim C54: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002
C57 \\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C57S \\sim C58S \\sim C59S \\sim C60S \\sim C61S \\sim C62S: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F36) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C57) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C60)
\\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C57S) \\sim Ueq, Uanis(C58S) \\sim Ueq, Uanis(C59S) \\sim Ueq,
Uanis(C60S) \\sim Ueq, Uanis(C61S) \\sim Ueq, Uanis(C62S) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(F1S)=Sof(F2S)=Sof(F3S)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(F7S)=Sof(F8S)=Sof(F9S)=1-FVAR(2)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(2)
 Sof(C57S)=Sof(H57S)=Sof(C58S)=Sof(H58S)=Sof(C59S)=Sof(H59S)=Sof(C60S)=
 Sof(H60S)=Sof(C61S)=Sof(H61S)=Sof(C62S)=Sof(H62S)=0.5*(1-FVAR(4))
 Sof(C57)=Sof(H57)=Sof(C58)=Sof(H58)=Sof(C59)=Sof(H59)=Sof(C60)=Sof(H60)=
 Sof(C61)=Sof(H61)=Sof(C62)=Sof(H62)=0.5*FVAR(4)
 Sof(F28S)=Sof(F29S)=Sof(F30S)=1-FVAR(4)
 Sof(F28)=Sof(F29)=Sof(F30)=FVAR(4)
5.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C25(H25), C28(H28)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C9(H9), C10(H10), C11(H11), C21(H21), C22(H22), C23(H23),
 C57(H57), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C57S(H57S),
 C58S(H58S), C59S(H59S), C60S(H60S), C61S(H61S), C62S(H62S)
5.c Fitted hexagon refined as free rotating group:
 C57(C58,C59,C60,C61,C62), C57S(C58S,C59S,C60S,C61S,C62S)
5.d 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              50511
_shelx_hkl_checksum              76773
_olex2_submission_special_instructions 'No special instructions were received'