GeCl<sub>x</sub>[Co(CO)<sub>3</sub>PR<sub>3</sub>]<sub>4-x</sub> (x = 0-3; R = <sup>n</sup>Pr, <sup>n</sup>Bu): from cobalt substituted germanes to novel binary cluster compounds.
Preißing, Lars; Behling, Elias; Schnepf, Andreas; Dalton transactions (Cambridge, England : 2003) 50 (2021) 10789–10797; doi:10.1039/d1dt02016a

data_7707838
_publ_section_title
;
 GeCl<sub>x</sub>[Co(CO)<sub>3</sub>PR<sub>3</sub>]<sub>4-x</sub> (x =
 0-3; R = <sup>n</sup>Pr, <sup>n</sup>Bu): from cobalt substituted
 germanes to novel binary cluster compounds.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10789
_journal_page_last               10797
_journal_paper_doi               10.1039/d1dt02016a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C108 H189 Co8 Ge7 O24 P7, 0.5[], 0.5[C4H8O], 0.5[C4H8O]'
_chemical_formula_sum            'C112 H197 Co8 Ge7 O25 P7'
_chemical_formula_weight         3140.04
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-12 deposited with the CCDC.	2021-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   19.3128(19)
_cell_length_b                   19.3128(19)
_cell_length_c                   22.471(3)
_cell_measurement_reflns_used    4103
_cell_measurement_temperature    150
_cell_measurement_theta_max      23.001
_cell_measurement_theta_min      2.183
_cell_volume                     7258.4(14)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 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 0.999
_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  0.1049
_diffrn_reflns_av_unetI/netI     0.0966
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            47737
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.386
_diffrn_reflns_theta_min         2.109
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.445
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1855 before and 0.0611 after correction. The Ratio of minimum to maximum transmission is 0.7794. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             3148
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.114
_refine_diff_density_max         0.828
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         9910
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1215
_refine_ls_R_factor_gt           0.0559
_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^)+(0.0697P)^2^+3.4927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1331
_refine_ls_wR_factor_ref         0.1647
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5504
_reflns_number_total             9910
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02016a2.cif
_cod_data_source_block           4_sq
_cod_depositor_comments
'Adding full bibliography for 7707835--7707841.cif.'
_cod_original_cell_volume        7258.5(18)
_cod_database_code               7707838
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C211-C213 = C212-C210 = C211-C210 = C210-C209
 1.54 with sigma of 0.02
 C310-C308 = C309-C307 = C314-C313 = C214-C212
 1.54 with sigma of 0.02
 C310-C308 \\sim C309-C307
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C307 \\sim C308: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C309 \\sim C310: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C211 \\sim C212: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C213 \\sim C214: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
4. Rigid body (RIGU) restrains
 C209, C210, C211, C212, C213, C214
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C311, C312, C313, C314, C315
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C305, C306, C307, C308, C309, C310
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H21C)=Sof(H21D)=Sof(C212)=Sof(H21G)=Sof(H21H)=Sof(C214)=Sof(H21L)=
 Sof(H21M)=Sof(H21N)=Sof(H30N)=Sof(H30O)=Sof(C307)=Sof(H30P)=Sof(H30Q)=
 Sof(C309)=Sof(H30T)=Sof(H30U)=Sof(H30V)=Sof(H31J)=Sof(H31K)=Sof(C315)=
 Sof(H31O)=Sof(H31P)=Sof(H31Q)=1-FVAR(1)
 Sof(H21A)=Sof(H21B)=Sof(C211)=Sof(H21E)=Sof(H21F)=Sof(C213)=Sof(H21I)=
 Sof(H21J)=Sof(H21K)=Sof(H30L)=Sof(H30M)=Sof(C308)=Sof(H30R)=Sof(H30S)=
 Sof(C310)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(H31H)=Sof(H31I)=Sof(C314)=
 Sof(H31L)=Sof(H31M)=Sof(H31N)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B), C102(H10C,H10D), C103(H10E,H10F), C201(H20A,H20B), C202(H20C,
 H20D), C203(H20E,H20F), C205(H20J,H20K), C206(H20L,H20M), C207(H20N,H20O),
 C209(H20S,H20T), C210(H21A,H21B), C210(H21C,H21D), C211(H21E,H21F), C212(H21G,
 H21H), C301(H30A,H30B), C302(H30C,H30D), C303(H30E,H30F), C305(H30J,H30K),
 C306(H30L,H30M), C306(H30N,H30O), C307(H30P,H30Q), C308(H30R,H30S), C311(H31D,
 H31E), C312(H31F,H31G), C313(H31J,H31K), C313(H31H,H31I)
6.b Me refined with riding coordinates:
 C309(H30T,H30U,H30V), C310(H31A,H31B,H31C), C314(H31L,H31M,H31N)
6.c Idealised Me refined as rotating group:
 C104(H10G,H10H,H10I), C204(H20G,H20H,H20I), C208(H20P,H20Q,H20R), C213(H21I,
 H21J,H21K), C214(H21L,H21M,H21N), C304(H30G,H30H,H30I), C315(H31O,H31P,H31Q)
;
_shelx_res_checksum              59032
_shelx_hkl_checksum              8958
_shelx_fab_checksum              48300
_platon_squeeze_special_details
;
A solvent mask was calculated and 88 electrons were found in a volume of 404\%A^3^ in 3 voids per unit cell.
This is consistent with the presence of 0.5[], 0.5[C4H8O], 0.5[C4H8O] per Formula Unit which account for 80 electrons per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'