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_7049049
_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         'C54 H40 Fe8 Ge6 O14, 4(C7 H8)'
_chemical_formula_sum            'C82 H72 Fe8 Ge6 O14'
_chemical_formula_weight         2163.73
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-09 deposited with the CCDC.    2019-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9394(10)
_cell_length_b                   20.9394(10)
_cell_length_c                   17.7553(19)
_cell_measurement_reflns_used    5696
_cell_measurement_temperature    150
_cell_measurement_theta_max      23.603
_cell_measurement_theta_min      2.459
_cell_volume                     7785.0(10)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_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 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  0.0545
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33705
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.497
_diffrn_reflns_theta_min         2.459
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    3.784
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1267 before and 0.0516 after correction. The Ratio of minimum to maximum transmission is 0.8180. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.846
_exptl_crystal_description       plate
_exptl_crystal_F_000             4304
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene, Et2O, pentane'
_exptl_crystal_size_max          0.226
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.117
_refine_diff_density_max         1.277
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4915
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0709P)^2^+48.0872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1540
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3483
_reflns_number_total             4915
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00097f2.cif
_cod_data_source_block           Ge6Fe8C82H72O14
_cod_original_cell_volume        7785.0(11)
_cod_database_code               7049049
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.666
_shelx_estimated_absorpt_t_min   0.482
_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
 C302-C307 = C307-C306 = C306-C305 = C305-C304 = C304-C303 = C303-C302
 1.4 with sigma of 0.02
 C302-C304 \\sim C302-C306 \\sim C303-C305 \\sim C307-C303 \\sim C306-C304
\\sim C307-C305
 with sigma of 0.04
 C301-C303 \\sim C301-C307
 with sigma of 0.04
3. Restrained planarity
 C301, C302, C303, C304, C305, C306, C307
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C301 \\sim C302 \\sim C303 \\sim C304 \\sim C305 \\sim C306 \\sim C307: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
5.a Aromatic/amide H refined with riding coordinates:
 C101(H101), C102(H102), C103(H103), C104(H104), C105(H105), C201(H201),
 C202(H202), C203(H203), C204(H204), C205(H205), C303(H303), C304(H304),
 C305(H305), C306(H306), C307(H307)
5.b Idealised Me refined as rotating group:
 C301(H30A,H30B,H30C)
;
_shelx_res_checksum              2444
_olex2_submission_special_instructions 'No special instructions were received'