On the reaction of GeCl2·Dioxane with KFeCp(CO)2: Isolation and characterization of novel bimetallic clusters
Schnepf, Andreas; Schrenk, Claudio; Preißing, Lars; Dalton Transactions  (2019) –; doi:10.1039/C9DT00097F

data_7049048
_publ_section_title
;
 On the reaction of GeCl2&#x00B7;Dioxane with KFeCp(CO)2: Isolation and
 characterization of novel bimetallic clusters
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT00097F
_journal_year                    2019
_chemical_formula_moiety         'C42 H30 Cl2 Fe6 Ge6 O12, 2(C4 H8 O)'
_chemical_formula_sum            'C50 H46 Cl2 Fe6 Ge6 O14'
_chemical_formula_weight         1712.41
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-04-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2018-11-09 deposited with the CCDC.    2019-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.141(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6575(9)
_cell_length_b                   21.880(2)
_cell_length_c                   22.8176(18)
_cell_measurement_reflns_used    9580
_cell_measurement_temperature    150
_cell_measurement_theta_max      31.450
_cell_measurement_theta_min      2.584
_cell_volume                     5796.6(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w 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  0.0480
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            147873
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.210
_diffrn_reflns_theta_min         1.792
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    4.667
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.4360
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1307 before and 0.0530 after correction. The Ratio of minimum to maximum transmission is 0.5841. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.962
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             3360
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene, Et2O, pentane'
_exptl_crystal_size_max          0.365
_exptl_crystal_size_mid          0.239
_exptl_crystal_size_min          0.056
_refine_diff_density_max         1.168
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.491(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         22110
_refine_ls_number_restraints     134
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0391P)^2^+7.8106P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0783
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                20188
_reflns_number_total             22110
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00097f2.cif
_cod_data_source_block           Ge6Fe6C50H46Cl2O14
_cod_original_cell_volume        5796.6(9)
_cod_database_code               7049048
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.509(8)
 0.491(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 C110-C109 \\sim C109-C108 \\sim C108-C107
 with sigma of 0.02
 O106-C110 \\sim O106-C107
 with sigma of 0.02
 O106-C109 \\sim O106-C108
 with sigma of 0.04
 C109-C107 \\sim C110-C108
 with sigma of 0.04
 C102-C103 \\sim C103-C104 \\sim C104-C105
 with sigma of 0.02
 O101-C102 \\sim O101-C105
 with sigma of 0.02
 O101-C103 \\sim O101-C104
 with sigma of 0.04
 C103-C105 \\sim C102-C104
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
O106 \\sim C107 \\sim C108 \\sim C109 \\sim C110: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
O101 \\sim C102 \\sim C103 \\sim C104 \\sim C105: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 O106, C107, C108, C109, C110
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O101, C102, C103, C104, C105
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 C102(H10A,H10B), C103(H10C,H10D), C104(H10E,H10F), C105(H10G,H10H), C107(H10I,
 H10J), C108(H10K,H10L), C109(H10M,H10N), C110(H11A,H11B)
6.b Aromatic/amide H refined with riding coordinates:
 C1F(H1F), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C21(H21),
 C22(H22), C23(H23), C24(H24), C25(H25), C31(H31), C32(H32), C33(H33), C34(H34),
  C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C51(H51), C52(H52),
 C53(H53), C54(H54), C55(H55), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65)
;
_shelx_res_checksum              81636
_olex2_submission_special_instructions 'No special instructions were received'