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_7049051
_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 Fe6 Ge6 O12, 3(C7 H8)'
_chemical_formula_sum            'C63 H54 Fe6 Ge6 O12'
_chemical_formula_weight         1773.70
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-12-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-11-09 deposited with the CCDC.    2019-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.2250(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.133(2)
_cell_length_b                   11.6457(8)
_cell_length_c                   19.5361(15)
_cell_measurement_reflns_used    6865
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.419
_cell_measurement_theta_min      2.168
_cell_volume                     6602.6(8)
_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      150.1
_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  0.0416
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29701
_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         30.517
_diffrn_reflns_theta_min         1.884
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    4.021
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0942 before and 0.0460 after correction. The Ratio of minimum to maximum transmission is 0.6919. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_description       block
_exptl_crystal_F_000             3504
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene, Et2O, pentane'
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.148
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         10079
_refine_ls_number_restraints     430
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0520P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1094
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6710
_reflns_number_total             10079
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00097f2.cif
_cod_data_source_block           Ge6Fe6C63H54O12
_cod_original_cell_volume        6602.7(8)
_cod_database_code               7049051
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.588
_shelx_estimated_absorpt_t_min   0.303
_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
 C401-C402
 1.51 with sigma of 0.02
 C415-C416
 1.51 with sigma of 0.02
 C417-C416 = C418-C417 = C419-C418 = C420-C419 = C412-C411 = C411-C410 = C410-
 C409 = C421-C416 = C414-C409 = C414-C413 = C421-C420 = C413-C412
 1.41 with sigma of 0.02
 C408-C409
 1.51 with sigma of 0.02
3. Restrained planarity
 C401, C402, C403, C404, C405, C406, C407
 with sigma of 0.1
 C415, C416, C417, C418, C419, C420, C421
 with sigma of 0.1
 C111, C112, C113, C114, C115
 with sigma of 0.1
 C211, C212, C213, C214, C215
 with sigma of 0.1
 C408, C409, C410, C411, C412, C413, C414
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C401 \\sim C402 \\sim C403 \\sim C404 \\sim C405 \\sim C406 \\sim C407: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C415 \\sim C416 \\sim C417 \\sim C418 \\sim C419 \\sim C420 \\sim C421: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C111 \\sim C112 \\sim C113 \\sim C114 \\sim C115: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
C211 \\sim C212 \\sim C213 \\sim C214 \\sim C215: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
C408 \\sim C411 \\sim C412 \\sim C413 \\sim C414: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
Uanis(C418) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C410) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C201, C202, C203, C204, C205
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C101, C102, C103, C104, C105
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C401, C402, C403, C404, C405, C406, C407
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C415, C416, C417, C418, C419, C420, C421
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C111, C112, C113, C114, C115
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C211, C212, C213, C214, C215
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C408, C411, C412, C413, C414
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C111)=Sof(H111)=Sof(C112)=Sof(H112)=Sof(C113)=Sof(H113)=Sof(C114)=
 Sof(H114)=Sof(C115)=Sof(H115)=Sof(C211)=Sof(H211)=Sof(C212)=Sof(H212)=
 Sof(C213)=Sof(H213)=Sof(C214)=Sof(H214)=Sof(C215)=Sof(H215)=Sof(C408)=
 Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C411)=Sof(H411)=Sof(C412)=Sof(H412)=
 Sof(C413)=Sof(H413)=Sof(C414)=Sof(H414)=Sof(C409)=Sof(C410)=Sof(H410)=1-FVAR(1)
 Sof(C101)=Sof(H101)=Sof(C102)=Sof(H102)=Sof(C103)=Sof(H103)=Sof(C104)=
 Sof(H104)=Sof(C105)=Sof(H105)=Sof(C201)=Sof(H201)=Sof(C202)=Sof(H202)=
 Sof(C203)=Sof(H203)=Sof(C204)=Sof(H204)=Sof(C205)=Sof(H205)=Sof(C415)=
 Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C416)=Sof(C417)=Sof(H417)=Sof(C418)=
 Sof(H418)=Sof(C419)=Sof(H419)=Sof(C420)=Sof(H420)=Sof(C421)=Sof(H421)=FVAR(1)
 Fixed Sof: C401(0.5) H40D(0.5) H40E(0.5) H40F(0.5) C402(0.5) C403(0.5)
 H403(0.5) C404(0.5) H404(0.5) C405(0.5) H405(0.5) C406(0.5) H406(0.5)
 C407(0.5) H407(0.5)
7.a Me refined with riding coordinates:
 C415(H41A,H41B,H41C)
7.b Aromatic/amide H refined with riding coordinates:
 C301(H301), C302(H302), C303(H303), C304(H304), C305(H305), C101(H101),
 C102(H102), C103(H103), C104(H104), C105(H105), C201(H201), C202(H202),
 C203(H203), C204(H204), C205(H205), C111(H111), C112(H112), C113(H113),
 C114(H114), C115(H115), C211(H211), C212(H212), C213(H213), C214(H214),
 C215(H215), C417(H417), C418(H418), C419(H419), C420(H420), C421(H421),
 C411(H411), C412(H412), C413(H413), C414(H414), C410(H410), C403(H403),
 C404(H404), C405(H405), C406(H406), C407(H407)
7.c Fitted hexagon refined as free rotating group:
 C416(C417,C418,C419,C420,C421), C411(C412,C413,C414,C409,C410), C402(C403,
 C404,C405,C406,C407)
7.d Idealised Me refined as rotating group:
 C408(H40A,H40B,H40C), C401(H40D,H40E,H40F)
;
_shelx_res_checksum              8538
_olex2_submission_special_instructions 'No special instructions were received'