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_7707839
_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         'C45 H81 Cl Co3 Ge O9 P3'
_chemical_formula_sum            'C45 H81 Cl Co3 Ge O9 P3'
_chemical_formula_weight         1143.83
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_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            8
_cell_length_a                   43.184(3)
_cell_length_b                   12.2679(8)
_cell_length_c                   21.4813(13)
_cell_measurement_reflns_used    6090
_cell_measurement_temperature    150
_cell_measurement_theta_max      19.321
_cell_measurement_theta_min      2.378
_cell_volume                     11380.3(13)
_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 0.998
_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  0.1102
_diffrn_reflns_av_unetI/netI     0.1026
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            102875
_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         26.376
_diffrn_reflns_theta_min         1.909
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.559
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6070
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1228 before and 0.0759 after correction. The Ratio of minimum to maximum transmission is 0.8143. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       block
_exptl_crystal_F_000             4784
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
;
 Flack x determined using 5491 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1211
_refine_ls_number_reflns         23226
_refine_ls_number_restraints     297
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0415P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1270
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                15319
_reflns_number_total             23226
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02016a2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7707835--7707841.cif.'
_cod_original_cell_volume        11380.2(12)
_cod_database_code               7707839
_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
 C614-C613 = C615-C614 = C616-C615 = C612-C611 = C611-C610 = C610-C609
 1.54 with sigma of 0.02
 C608-C607 = C602-C607 = C602-C601
 1.54 with sigma of 0.02
 C619-C623 = C622-C623 = C619-C618 = C622-C618 = C617-C618 = C621-C618 = C602-
 C601 = C602-C607 = C608-C607
 1.54 with sigma of 0.02
 C619-C620 = C623-C622
 1.54 with sigma of 0.02
 C613-C615
 2.54 with sigma of 0.04
 C609-C611
 2.54 with sigma of 0.04
 C613-C614 \\sim C614-C615
 with sigma of 0.02
 C609-C610 \\sim C610-C611
 with sigma of 0.02
 C613-C615 \\sim C614-C616
 with sigma of 0.02
 C609-C611 \\sim C610-C612
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C617 \\sim C621: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C613 \\sim C614 \\sim C615: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C609 \\sim C610 \\sim C611: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C609 \\sim C610 \\sim C611 \\sim C612 \\sim C613 \\sim C614 \\sim C615 \\sim
C616: within 6A with sigma of 0.01 and sigma for terminal atoms of 0.02
C601 \\sim C605: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C602 \\sim C606: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C603 \\sim C607: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C604 \\sim C608: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C620 \\sim C623: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C619) \\sim Ueq, Uanis(C622) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C607) \\sim Ueq, Uanis(C601) \\sim Ueq, Uanis(C602) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C623) \\sim Ueq, Uanis(C620) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C613, C614, C615
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C609, C610, C611
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C601, C602, C607, C608
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C605)=Sof(H60N)=Sof(H60O)=Sof(C606)=Sof(H60L)=Sof(H60M)=Sof(C607)=
 Sof(H60E)=Sof(H60F)=Sof(C608)=Sof(H60G)=Sof(H60H)=Sof(H60I)=Sof(C613)=
 Sof(H61H)=Sof(H61I)=Sof(C614)=Sof(H61J)=Sof(H61K)=Sof(C615)=Sof(H61L)=
 Sof(H61M)=Sof(C616)=Sof(H61N)=Sof(H61O)=Sof(H61P)=Sof(H61U)=Sof(H61V)=
 Sof(C619)=Sof(H61W)=Sof(H61X)=Sof(C620)=Sof(H62H)=Sof(H62I)=Sof(H62J)=
 Sof(C621)=Sof(H62A)=Sof(H62B)=1-FVAR(1)
 Sof(C601)=Sof(H60A)=Sof(H60B)=Sof(C602)=Sof(H60C)=Sof(H60D)=Sof(C603)=
 Sof(H60P)=Sof(H60Q)=Sof(C604)=Sof(H60R)=Sof(H60S)=Sof(H60T)=Sof(C609)=
 Sof(H60J)=Sof(H60K)=Sof(C610)=Sof(H61A)=Sof(H61B)=Sof(C611)=Sof(H61C)=
 Sof(H61D)=Sof(C612)=Sof(H61E)=Sof(H61F)=Sof(H61G)=Sof(C617)=Sof(H61Q)=
 Sof(H61R)=Sof(H61S)=Sof(H61T)=Sof(C622)=Sof(H62C)=Sof(H62D)=Sof(C623)=
 Sof(H62E)=Sof(H62F)=Sof(H62G)=FVAR(1)
6.a Free rotating group:
 C609(C610,C611), C613(C614,C615)
6.b Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B), C102(H10C,H10D), C103(H10E,H10F), C105(H10J,H10K), C106(H10L,
 H10M), C107(H10N,H10O), C109(H10S,H10T), C110(H11A,H11B), C111(H11C,H11D),
 C201(H20A,H20B), C202(H20C,H20D), C203(H20E,H20F), C205(H20J,H20K), C206(H20L,
 H20M), C207(H20N,H20O), C209(H20S,H20T), C210(H21A,H21B), C211(H21C,H21D),
 C301(H30A,H30B), C302(H30C,H30D), C303(H30E,H30F), C305(H30J,H30K), C306(H30L,
 H30M), C307(H30N,H30O), C309(H30S,H30T), C310(H31A,H31B), C311(H31C,H31D),
 C401(H40A,H40B), C402(H40C,H40D), C403(H40E,H40F), C405(H40J,H40K), C406(H40L,
 H40M), C407(H40N,H40O), C409(H40S,H40T), C410(H41A,H41B), C411(H41C,H41D),
 C501(H50A,H50B), C502(H50C,H50D), C503(H50E,H50F), C505(H50J,H50K), C506(H50L,
 H50M), C507(H50N,H50O), C509(H50S,H50T), C510(H51A,H51B), C511(H51C,H51D),
 C601(H60A,H60B), C602(H60C,H60D), C603(H60P,H60Q), C605(H60N,H60O), C606(H60L,
 H60M), C607(H60E,H60F), C609(H60J,H60K), C610(H61A,H61B), C611(H61C,H61D),
 C613(H61H,H61I), C614(H61J,H61K), C615(H61L,H61M), C617(H61Q,H61R), C618(H61U,
 H61V), C618(H61S,H61T), C619(H61W,H61X), C621(H62A,H62B), C622(H62C,H62D)
6.c Me refined with riding coordinates:
 C104(H10G,H10H,H10I), C108(H10P,H10Q,H10R), C112(H11E,H11F,H11G), C204(H20G,
 H20H,H20I), C208(H20P,H20Q,H20R), C212(H21E,H21F,H21G), C304(H30G,H30H,H30I),
 C308(H30P,H30Q,H30R), C312(H31E,H31F,H31G), C404(H40G,H40H,H40I), C408(H40P,
 H40Q,H40R), C412(H41E,H41F,H41G), C504(H50G,H50H,H50I), C508(H50P,H50Q,H50R),
 C512(H51E,H51F,H51G), C604(H60R,H60S,H60T), C608(H60G,H60H,H60I), C612(H61E,
 H61F,H61G), C616(H61N,H61O,H61P), C620(H62H,H62I,H62J), C623(H62E,H62F,H62G)
;
_shelx_res_checksum              39224
_shelx_hkl_checksum              57477
_olex2_submission_special_instructions 'No special instructions were received'