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_7707841
_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         'C24 H42 Cl2 Co2 Ge O6 P2'
_chemical_formula_sum            'C24 H42 Cl2 Co2 Ge O6 P2'
_chemical_formula_weight         749.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 101.607(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8319(15)
_cell_length_b                   18.047(2)
_cell_length_c                   17.997(2)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.547
_cell_measurement_theta_min      2.226
_cell_volume                     3446.2(7)
_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      150.01
_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 0.995
_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  0.0574
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            78968
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.610
_diffrn_reflns_theta_min         2.227
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.098
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1448 before and 0.0498 after correction. The Ratio of minimum to maximum transmission is 0.8668. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       plank
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.845
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         10572
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0379P)^2^+1.1061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7900
_reflns_number_total             10572
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02016a2.cif
_cod_data_source_block           69
_cod_depositor_comments
'Adding full bibliography for 7707835--7707841.cif.'
_cod_original_cell_volume        3446.3(8)
_cod_database_code               7707841
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Others
 Sof(C104)=Sof(H10H)=Sof(H10I)=Sof(C105)=Sof(H10J)=Sof(H10K)=Sof(C106)=
 Sof(H10L)=Sof(H10M)=Sof(H10N)=Sof(C107)=Sof(H10O)=Sof(H10P)=Sof(C108)=
 Sof(H10Q)=Sof(H10R)=Sof(H10V)=Sof(H10W)=Sof(H10X)=Sof(H11L)=Sof(H11M)=
 Sof(H11N)=Sof(C115)=Sof(H11O)=Sof(H11P)=Sof(C116)=Sof(H11Q)=Sof(H11R)=1-FVAR(1)
 Sof(C101)=Sof(H10A)=Sof(H10B)=Sof(C102)=Sof(H10C)=Sof(H10D)=Sof(C103)=
 Sof(H10E)=Sof(H10F)=Sof(H10G)=Sof(H10S)=Sof(H10T)=Sof(H10U)=Sof(C110)=
 Sof(H11A)=Sof(H11B)=Sof(C111)=Sof(H11C)=Sof(H11D)=Sof(C112)=Sof(H11E)=
 Sof(H11F)=Sof(C113)=Sof(H11G)=Sof(H11H)=Sof(H11I)=Sof(H11J)=Sof(H11K)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B), C102(H10C,H10D), C104(H10H,H10I), C105(H10J,H10K), C107(H10O,
 H10P), C108(H10Q,H10R), C110(H11A,H11B), C111(H11C,H11D), C112(H11E,H11F),
 C113(H11G,H11H), C115(H11O,H11P), C116(H11Q,H11R), C201(H20A,H20B), C202(H20C,
 H20D), C204(H20H,H20I), C205(H20J,H20K), C207(H20O,H20P), C208(H20Q,H20R)
3.b Idealised Me refined as rotating group:
 C103(H10E,H10F,H10G), C106(H10L,H10M,H10N), C109(H10S,H10T,H10U), C109(H10V,
 H10W,H10X), C114(H11I,H11J,H11K), C114(H11L,H11M,H11N), C203(H20E,H20F,H20G),
 C206(H20L,H20M,H20N), C209(H20S,H20T,H20U)
;
_shelx_res_checksum              39696
_shelx_hkl_checksum              8981
_olex2_submission_special_instructions 'No special instructions were received'