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_7707836
_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         'C48 H84 Co4 Ge1 O12 P4'
_chemical_formula_sum            'C48 H84 Co4 Ge O12 P4'
_chemical_formula_weight         1285.34
_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_Hall           'P 2ac 2ab 3'
_space_group_name_H-M_alt        'P 21 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-17 deposited with the CCDC.	2021-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   28.9936(6)
_cell_length_b                   28.9936(6)
_cell_length_c                   28.9936(6)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.957
_cell_measurement_theta_min      2.221
_cell_volume                     24372.9(9)
_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      150.01
_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 1.000
_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  0.0791
_diffrn_reflns_av_unetI/netI     0.0733
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            96962
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.278
_diffrn_reflns_theta_min         0.702
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.710
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6460
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0757 before and 0.0623 after correction. The Ratio of minimum to maximum transmission is 0.8663. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description       tetrahedron
_exptl_crystal_F_000             10688
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.345
_exptl_crystal_size_min          0.339
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 5701 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.073(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     931
_refine_ls_number_reflns         20218
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0575P)^2^+24.7100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1370
_reflns_Friedel_coverage         0.892
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                15220
_reflns_number_total             20218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02016a2.cif
_cod_data_source_block           88
_cod_depositor_comments
'Adding full bibliography for 7707835--7707841.cif.'
_cod_original_cell_volume        24372.9(15)
_cod_database_code               7707836
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.595
_shelx_estimated_absorpt_t_min   0.590
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8993(12)
 0.1007(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
C211 \\sim C231: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C212 \\sim C232: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C213 \\sim C233: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C214 \\sim C234: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C215 \\sim C235: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C216 \\sim C236: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C218 \\sim C238: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C217) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C217, C218, C219
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C231)=Sof(H23A)=Sof(H23B)=Sof(C232)=Sof(H23C)=Sof(H23D)=Sof(C233)=
 Sof(H23E)=Sof(H23F)=Sof(H23G)=Sof(C234)=Sof(H23H)=Sof(H23I)=Sof(C235)=
 Sof(H23J)=Sof(H23K)=Sof(C236)=Sof(H23L)=Sof(H23M)=Sof(H23N)=Sof(C237)=
 Sof(H23O)=Sof(H23P)=Sof(C238)=Sof(H23Q)=Sof(H23R)=Sof(C239)=Sof(H23S)=
 Sof(H23T)=Sof(H23U)=1-FVAR(1)
 Sof(C211)=Sof(H21A)=Sof(H21B)=Sof(C212)=Sof(H21C)=Sof(H21D)=Sof(C213)=
 Sof(H21E)=Sof(H21F)=Sof(H21G)=Sof(C214)=Sof(H21H)=Sof(H21I)=Sof(C215)=
 Sof(H21J)=Sof(H21K)=Sof(C216)=Sof(H21L)=Sof(H21M)=Sof(H21N)=Sof(C217)=
 Sof(H21O)=Sof(H21P)=Sof(C218)=Sof(H21Q)=Sof(H21R)=Sof(C219)=Sof(H21S)=
 Sof(H21T)=Sof(H21U)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C111(H11A,H11B), C112(H11C,H11D), C114(H11H,H11I), C115(H11J,H11K), C117(H11O,
 H11P), C118(H11Q,H11R), C121(H12A,H12B), C122(H12C,H12D), C211(H21A,H21B),
 C212(H21C,H21D), C214(H21H,H21I), C215(H21J,H21K), C217(H21O,H21P), C218(H21Q,
 H21R), C221(H22A,H22B), C222(H22C,H22D), C231(H23A,H23B), C232(H23C,H23D),
 C234(H23H,H23I), C235(H23J,H23K), C237(H23O,H23P), C238(H23Q,H23R), C311(H31A,
 H31B), C312(H31C,H31D), C314(H31H,H31I), C315(H31J,H31K), C317(H31O,H31P),
 C318(H31Q,H31R), C321(H32A,H32B), C322(H32C,H32D), C411(H41A,H41B), C412(H41C,
 H41D), C414(H41H,H41I), C415(H41J,H41K), C417(H41O,H41P), C418(H41Q,H41R),
 C421(H42A,H42B), C422(H42C,H42D)
6.b Idealised Me refined as rotating group:
 C113(H11E,H11F,H11G), C116(H11L,H11M,H11N), C119(H11S,H11T,H11U), C123(H12E,
 H12F,H12G), C213(H21E,H21F,H21G), C216(H21L,H21M,H21N), C219(H21S,H21T,H21U),
 C223(H22E,H22F,H22G), C233(H23E,H23F,H23G), C236(H23L,H23M,H23N), C239(H23S,
 H23T,H23U), C313(H31E,H31F,H31G), C316(H31L,H31M,H31N), C319(H31S,H31T,H31U),
 C323(H32E,H32F,H32G), C413(H41E,H41F,H41G), C416(H41L,H41M,H41N), C419(H41S,
 H41T,H41U), C423(H42E,H42F,H42G)
;
_shelx_res_checksum              75844
_shelx_hkl_checksum              14479
_olex2_submission_special_instructions 'No special instructions were received'