The influence of the FeCp(CO)<sub>2</sub><sup>+</sup> moiety on the dynamics of the metalloid [Ge<sub>9</sub>(Si(SiMe<sub>3</sub>)<sub>3</sub>)<sub>3</sub>]<sup>-</sup> cluster in thf: synthesis and characterization by time-resolved absorption spectroscopy.
Michenfelder, Nadine C.; Gienger, Christian; Schnepf, Andreas; Unterreiner, Andreas-Neil; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15577–15582; doi:10.1039/c9dt02091h

data_7700663
_publ_section_title
;
 The influence of the FeCp(CO)<sub>2</sub><sup>+</sup> moiety on the
 dynamics of the metalloid
 [Ge<sub>9</sub>(Si(SiMe<sub>3</sub>)<sub>3</sub>)<sub>3</sub>]<sup>-</sup>
 cluster in thf: synthesis and characterization by time-resolved
 absorption spectroscopy.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15577
_journal_page_last               15582
_journal_paper_doi               10.1039/c9dt02091h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C34 H86 Fe Ge9 O2 Si12'
_chemical_formula_sum            'C34 H86 Fe Ge9 O2 Si12'
_chemical_formula_weight         1573.26
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-06-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-20 deposited with the CCDC.    2019-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                89.905(2)
_cell_angle_beta                 85.864(2)
_cell_angle_gamma                78.757(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5603(5)
_cell_length_b                   14.6941(8)
_cell_length_c                   24.4867(13)
_cell_measurement_reflns_used    9979
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.526
_cell_measurement_theta_min      2.172
_cell_volume                     3364.8(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.01
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            182883
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.589
_diffrn_reflns_theta_min         1.650
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    4.407
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1438 before and 0.0631 after correction. The Ratio of minimum to maximum transmission is 0.6949. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       needle
_exptl_crystal_F_000             1576
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: thf, pentane, toluene'
_exptl_crystal_size_max          0.391
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         20621
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+0.4598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0859
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14578
_reflns_number_total             20621
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02091h2.cif
_cod_data_source_block           2
_cod_depositor_comments          'Adding full bibliography for 7700663.cif.'
_cod_database_code               7700663
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.857
_shelx_estimated_absorpt_t_min   0.278
_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. Uiso/Uaniso restraints and constraints
C12 \\sim C14 \\sim C16 \\sim C18 \\sim C20: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C11 \\sim C13 \\sim C15 \\sim C17 \\sim C19: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
3. Others
 Sof(C11)=Sof(H11)=Sof(C13)=Sof(H13)=Sof(C15)=Sof(H15)=Sof(C17)=Sof(H17)=
 Sof(C19)=Sof(H19)=1-FVAR(1)
 Sof(C12)=Sof(H12)=Sof(C14)=Sof(H14)=Sof(C16)=Sof(H16)=Sof(C18)=Sof(H18)=
 Sof(C20)=Sof(H20)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C16(H16), C18(H18), C20(H20), C11(H11), C13(H13),
 C15(H15), C17(H17), C19(H19)
4.b Idealised Me refined as rotating group:
 C201(H20A,H20B,H20C), C202(H20D,H20E,H20F), C203(H20G,H20H,H20I), C204(H20J,
 H20K,H20L), C205(H20M,H20N,H20O), C206(H20P,H20Q,H20R), C207(H20S,H20T,H20U),
 C208(H20V,H20W,H20X), C209(H20Y,H,HA), C301(H30A,H30B,H30C), C302(H30D,H30E,
 H30F), C303(H30G,H30H,H30I), C304(H30J,H30K,H30L), C305(H30M,H30N,H30O),
 C306(H30P,H30Q,H30R), C307(H30S,H30T,H30U), C308(H30V,H30W,H30X), C309(H30Y,HB,
 HC), C801(H80A,H80B,H80C), C802(H80D,H80E,H80F), C803(H80G,H80H,H80I),
 C804(H80J,H80K,H80L), C805(H80M,H80N,H80O), C806(H80P,H80Q,H80R), C807(H80S,
 H80T,H80U), C808(H80V,H80W,H80X), C809(H80Y,HD,HE)
;
_shelx_res_checksum              97131
_olex2_submission_special_instructions 'No special instructions were received'