[Co2@(Ge17Ni)]4−: The First Edge-Sharing Double-Cage Endohedral Germanide
Xu, Hong-Lei; Qiao, Lei; Sun, Zhong-Ming; Chemical Communications  (2022) –; doi:10.1039/D1CC06038D

data_7129700
_publ_section_title
;
 [Co2@(Ge17Ni)]4&#x2212;: The First Edge-Sharing Double-Cage Endohedral
 Germanide
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06038D
_journal_year                    2022
_chemical_formula_moiety         'Co2 Ge17 Ni, 4(C18 H36 K N2 O6)'
_chemical_formula_sum            'C72 H144 Co2 Ge17 K4 N8 Ni O24'
_chemical_formula_weight         3072.94
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-29
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-09-24 deposited with the CCDC.	2022-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6463(3)
_cell_length_b                   25.7355(5)
_cell_length_c                   28.7503(6)
_cell_measurement_reflns_used    9626
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.3190
_cell_measurement_theta_min      4.3280
_cell_volume                     12316.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (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(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.985
_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    -29.00  32.00   0.50    0.50    --    0.00 -82.00 150.00  122
  2  \w    -29.00  -3.00   0.50    0.50    --    0.00 -82.00-180.00   52
  3  \w     19.00  79.00   0.50    0.50    --    0.00  38.00 -30.00  120
  4  \w     -9.00  17.00   0.50    0.50    --    0.00  38.00 -30.00   52
  5  \w    -38.00  18.00   0.50    0.50    --    0.00 -82.00 -90.00  112
  6  \w     15.00 105.00   0.50    0.50    --  101.60 -57.00  60.00  180
  7  \w     32.00  68.00   0.50    0.50    --  101.60 -82.00   0.00   72
  8  \w     14.00 134.00   0.50    0.50    --  101.60 -82.00  60.00  240
  9  \w     89.00 114.00   0.50    0.50    --  101.60 -82.00 120.00   50
 10  \w     77.00 127.00   0.50    0.50    --  101.60 -82.00 -90.00  100
 11  \w     22.00  48.00   0.50    0.50    --  101.60 -82.00 -90.00   52
 12  \w     73.00 184.00   0.50    0.50    --  101.60  19.00 -30.00  222
 13  \w    100.00 126.00   0.50    0.50    --  101.60 -82.00-150.00   52
 14  \w    111.00 136.00   0.50    0.50    --  101.60  82.00-150.00   50
 15  \w     45.00 125.00   0.50    0.50    --  101.60 -26.00  99.00  160
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0053995000
_diffrn_orient_matrix_UB_12      -0.0563239000
_diffrn_orient_matrix_UB_13      0.0178787000
_diffrn_orient_matrix_UB_21      0.0924406000
_diffrn_orient_matrix_UB_22      -0.0036170000
_diffrn_orient_matrix_UB_23      0.0002163000
_diffrn_orient_matrix_UB_31      0.0013833000
_diffrn_orient_matrix_UB_32      0.0199073000
_diffrn_orient_matrix_UB_33      0.0504875000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0880
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            68568
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.999
_diffrn_reflns_theta_min         3.763
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    8.432
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic blackish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_description       plate
_exptl_crystal_F_000             6104
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         2.210
_refine_diff_density_min         -1.163
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         10979
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0771
_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^)+(0.1416P)^2^+18.0175P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2221
_refine_ls_wR_factor_ref         0.2433
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7407
_reflns_number_total             10979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06038d2.cif
_cod_data_source_block           xhl
_cod_database_code               7129700
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.258
_shelx_estimated_absorpt_t_min   0.218
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Shared sites
{Ni1, Ge}
3. Uiso/Uaniso restraints and constraints
Uanis(Ni1) = Uanis(Ge)
4. Others
 Fixed Sof: Ge01(0.5) Ge02(0.5) Ge00(0.5) Ge2A(0.5) Ge2(0.5) Ge3(0.5) Ge4(0.5)
 Ge5(0.5) Ge6(0.5) Ge7(0.5) Ge8(0.5) Ge1A(0.5) Ge0A(0.5) Ge3A(0.5) Ge10(0.5)
 Ge9(0.5) Ge(0.5) Ni1(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C00W(H00A,H00B), C00X(H00G,H00H), C00Y(H00C,H00D), C00Z(H00E,H00F), C010(H01A,
 H01B), C011(H01C,H01D), C012(H01E,H01F), C013(H01G,H01H), C014(H01I,H01J),
 C015(H0AA,H), C016(H01K,H01L), C017(H01M,H01N), C018(H01O,H01P), C019(H01Q,
 H01R), C01A(H01S,H01T), C01B(H01U,H01V), C01C(H01W,H01X), C01D(H01Y,HA),
 C01E(H1AA,HB), C01F(H2AA,HC), C01G(H01Z,HD), C01H(H3AA,HE), C01I(H01,HF),
 C01J(H4AA,HG), C01K(H5AA,HH), C01L(H6AA,HI), C01M(H7AA,HJ), C01N(H8AA,HK),
 C01O(H9AA,HL), C01P(H0BA,HM), C01Q(H1BA,HN), C01R(H2BA,HO), C01S(H3BA,HP),
 C01T(H4BA,HQ), C01U(H5BA,HR), C01V(H6BA,HS)
;
_shelx_res_checksum              42513
_shelx_hkl_checksum              98680
_shelx_fab_checksum              33804
_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 2.332
_oxdiff_exptl_absorpt_empirical_full_min 0.662