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_7707840
_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         'C36 H63 Cl Co3 Ge O9 P3, C4 H10 O'
_chemical_formula_sum            'C40 H73 Cl Co3 Ge O10 P3'
_chemical_formula_weight         1091.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-12 deposited with the CCDC.	2021-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.851(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.6499(2)
_cell_length_b                   14.5313(2)
_cell_length_c                   13.9137(2)
_cell_measurement_reflns_used    46230
_cell_measurement_temperature    100.00(14)
_cell_measurement_theta_max      45.4210
_cell_measurement_theta_min      2.2930
_cell_volume                     2641.29(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.79a (Rigaku OD, 2020)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(14)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -60.00 -35.00   0.50   31.08    --  -45.08 126.00 172.00   50
  2  \w     16.00  42.00   0.50   31.08    --   46.33-126.00  95.00   52
  3  \w    -24.00   2.00   0.50   31.08    --  -45.08  57.00 -90.00   52
  4  \w    -94.00 -39.00   0.50   31.08    --  -45.08 131.00  96.82  110
  5  \w    -46.00 -10.00   0.50   31.08    --  -45.08  77.00 -30.00   72
  6  \w    -46.00  18.00   0.50   31.08    --  -45.08  19.00 -60.00  128
  7  \w    -88.00 -38.00   0.50   31.08    --  -45.08 118.00  22.73  100
  8  \w    -25.00  34.00   0.50   31.08    --  -45.08  19.00  30.00  118
  9  \w    -98.00 -62.00   0.50   31.08    --  -45.08 137.00 106.81   72
 10  \w   -106.00 -37.00   0.50   31.08    --  -45.08 -37.00 -30.00  138
 11  \w   -104.00 -39.00   0.50   31.08    --  -45.08 -37.00 120.00  130
 12  \w    -94.00 -69.00   0.50   31.08    --  -45.08 131.00  45.15   50
 13  \w    -51.00 -25.00   0.50   31.08    --  -45.08  37.00 -30.00   52
 14  \w      5.00  30.00   0.50   31.08    --  -45.08  37.00 -30.00   50
 15  \w      0.00  34.00   0.50   31.08    --  -45.08  19.00-120.00   68
 16  \w    -57.00 -31.00   0.50   31.08    --  -45.08  57.00 -90.00   52
 17  \w    -31.00   5.00   0.50   31.08    --   46.33 -19.00 -90.00   72
 18  \w    -31.00   5.00   0.50   31.08    --   46.33 -19.00 -30.00   72
 19  \w    -10.00  31.00   0.50   31.08    --    0.62  57.00 120.00   82
 20  \w   -118.00 -85.00   0.50   31.08    --  -45.08 -52.00 -77.09   66
 21  \w    -56.00 -31.00   0.50   31.08    --  -45.08 -60.00-145.68   50
 22  \w    -56.00 -31.00   0.50   31.08    --  -45.08 -60.00  49.95   50
 23  \w   -100.00 -65.00   0.50   31.08    --  -45.08 -51.00 -34.27   70
 24  \w    -61.00 -35.00   0.50   31.08    --  -45.08 -51.00 -34.27   52
 25  \w    -74.00 -34.00   0.50   31.08    --  -45.08 -52.00 -77.09   80
 26  \w    -58.00 -32.00   0.50   31.08    --  -45.08 -58.00-119.60   52
 27  \w    -59.00 -33.00   0.50   31.08    --  -45.08 -55.00-111.25   52
 28  \w    -59.00 -33.00   0.50   31.08    --  -45.08 -55.00  -5.89   52
 29  \w   -116.00 -78.00   0.50   31.08    --  -45.08 -52.00 108.34   76
 30  \w    -65.00 -34.00   0.50   31.08    --  -45.08 -52.00 108.34   62
 31  \w    -57.00 -32.00   0.50   31.08    --  -45.08 -58.00  70.75   50
 32  \w    -60.00 -34.00   0.50   31.08    --  -45.08 -54.00  17.19   52
 33  \w    -58.00 -32.00   0.50   31.08    --  -45.08 -59.00-169.42   52
 34  \w    -59.00 -33.00   0.50   31.08    --  -45.08 -56.00 -41.59   52
 35  \w    -95.00 -43.00   0.50   31.08    --  -45.08 133.00 -91.22  104
 36  \w    -53.00  32.00   0.50   31.08    --  -45.08  37.00 150.00  170
 37  \w    -95.00 -42.00   0.50   31.08    --  -45.08 133.00-129.77  106
 38  \w    -50.00  30.00   0.50   31.08    --  -45.08  37.00-150.00  160
 39  \w   -113.00 -35.00   0.50   31.08    --  -45.08 -47.00  67.84  156
 40  \w    -98.00 -40.00   0.50   31.08    --  -45.08 -50.00 156.94  116
 41  \w    -93.00 -40.00   0.50   31.08    --  -45.08 130.00 -16.24  106
 42  \w    -33.00  34.00   0.50   31.08    --  -45.08  19.00  60.00  134
 43  \w   -117.00 -34.00   0.50   31.08    --  -45.08 -51.00-142.88  166
 44  \w    -60.00 -33.00   0.50   31.08    --  -45.08 -56.00 144.96   54
 45  \w    -48.00  21.00   0.50   31.08    --  -45.08  19.00 150.00  138
 46  \w    -26.00  26.00   0.50   31.08    --   46.33 -57.00-150.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0384843000
_diffrn_orient_matrix_UB_12      -0.0337875000
_diffrn_orient_matrix_UB_13      0.0179308000
_diffrn_orient_matrix_UB_21      0.0358078000
_diffrn_orient_matrix_UB_22      0.0350816000
_diffrn_orient_matrix_UB_23      0.0213671000
_diffrn_orient_matrix_UB_31      -0.0135980000
_diffrn_orient_matrix_UB_32      -0.0031977000
_diffrn_orient_matrix_UB_33      0.0453733000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0873
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            176659
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.500
_diffrn_reflns_theta_min         2.074
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.677
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.787
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.79a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       plate
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 9032 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         24143
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0149P)^2^+0.8018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0645
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                21199
_reflns_number_total             24143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02016a2.cif
_cod_data_source_block           1001
_cod_depositor_comments
'Adding full bibliography for 7707835--7707841.cif.'
_cod_database_code               7707840
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C80 H146 Cl2 Co6 Ge2 O20 P6'
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.811
_diffrn_oxdiff_digest_frames
;
01069a217aef9a6202b272f35f2eb8d26203902b85f
;
_diffrn_oxdiff_digest_hkl
;
018c0ba13d74e666bded72d623499990c8612c
;
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     45.18
_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
2.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), C201(H20A,H20B), C202(H20C,H20D), C204(H20H,H20I),
 C205(H20J,H20K), C207(H20O,H20P), C208(H20Q,H20R), C301(H30A,H30B), C302(H30C,
 H30D), C304(H30H,H30I), C305(H30J,H30K), C307(H30O,H30P), C308(H30Q,H30R),
 C402(H40D,H40E), C404(H40F,H40G)
2.b Idealised Me refined as rotating group:
 C103(H10E,H10F,H10G), C106(H10L,H10M,H10N), C109(H10S,H10T,H10U), C203(H20E,
 H20F,H20G), C206(H20L,H20M,H20N), C209(H20S,H20T,H20U), C303(H30E,H30F,H30G),
 C306(H30L,H30M,H30N), C309(H30S,H30T,H30U), C401(H40A,H40B,H40C), C405(H40H,
 H40I,H40J)
;
_shelx_res_checksum              10221
_shelx_hkl_checksum              43725
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.544
_oxdiff_exptl_absorpt_empirical_full_min 0.741