Metalloid germanium cluster shears for lanthanide diiodides
Klementyeva, Svetlana; Schrenk, Claudio; Zhang, Minghui; Khusniyarov, Marat M.; Dalton Transactions  (2023) –; doi:10.1039/D3DT00578J

data_7712680
_publ_section_title
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 Metalloid germanium cluster shears for lanthanide diiodides
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00578J
_journal_year                    2023
_chemical_compound_source        thf
_chemical_formula_moiety         'C32 H64 I2 O8 Yb2, 2(C27 H81 Ge9 Si12)'
_chemical_formula_sum            'C86 H226 Ge18 I2 O8 Si24 Yb2'
_chemical_formula_weight         3969.31
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-28
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-13 deposited with the CCDC.	2023-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.373(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.1512(8)
_cell_length_b                   24.1678(14)
_cell_length_c                   25.8345(15)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    150
_cell_measurement_theta_max      21.079
_cell_measurement_theta_min      2.240
_cell_volume                     8820.2(9)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0967
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            235660
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.393
_diffrn_reflns_theta_min         1.602
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    4.611
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1488 before and 0.0640 after correction. The Ratio of minimum to maximum transmission is 0.6159. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       block
_exptl_crystal_F_000             3928
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.284
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.047
_refine_diff_density_max         1.152
_refine_diff_density_min         -1.142
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     713
_refine_ls_number_reflns         18057
_refine_ls_number_restraints     404
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0470P)^2^+19.9041P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1123
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12331
_reflns_number_total             18057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00578j2.cif
_cod_data_source_block           8_sq
_cod_database_code               7712680
_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
2. Restrained distances
 C420-C419 \\sim C419-C418 \\sim C418-C417
 with sigma of 0.02
 O416-C420 \\sim O416-C417
 with sigma of 0.02
 O416-C419 \\sim O416-C418
 with sigma of 0.04
 C419-C417 \\sim C420-C418
 with sigma of 0.04
 C415-C414 \\sim C414-C408 \\sim C408-C412
 with sigma of 0.02
 O411-C415 \\sim O411-C412
 with sigma of 0.02
 O411-C414 \\sim O411-C408
 with sigma of 0.04
 C414-C412 \\sim C415-C408
 with sigma of 0.04
 C425-C424 \\sim C424-C423 \\sim C423-C422
 with sigma of 0.02
 O421-C425 \\sim O421-C422
 with sigma of 0.02
 O421-C424 \\sim O421-C423
 with sigma of 0.04
 C424-C422 \\sim C425-C423
 with sigma of 0.04
 C410-C409 \\sim C409-C413 \\sim C413-C407
 with sigma of 0.02
 O406-C410 \\sim O406-C407
 with sigma of 0.02
 O406-C409 \\sim O406-C413
 with sigma of 0.04
 C409-C407 \\sim C410-C413
 with sigma of 0.04
 Yb1-O416 \\sim Yb1-O421
 with sigma of 0.02
 Yb1-O411 \\sim Yb1-O406
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O416 \\sim C417 \\sim C418 \\sim C419 \\sim C420: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
O411 \\sim C408 \\sim C412 \\sim C414 \\sim C415: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
O421 \\sim C422 \\sim C423 \\sim C424 \\sim C425: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
O406 \\sim C407 \\sim C409 \\sim C410 \\sim C413: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
O416 \\sim O421: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C418 \\sim C423: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O406 \\sim O411: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C407 \\sim C412: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C408 \\sim C413: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C409 \\sim C414: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C410 \\sim C415: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C402) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C420) \\sim Ueq, Uanis(C425) \\sim Ueq, Uanis(C419) \\sim Ueq,
Uanis(C424) \\sim Ueq, Uanis(C418) \\sim Ueq, Uanis(C423) \\sim Ueq,
Uanis(C422) \\sim Ueq, Uanis(C417) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C410) \\sim Ueq, Uanis(C415) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O401, C402, C403, C404, C405
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O416, C417, C418, C419, C420
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O411, C408, C412, C414, C415
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O421, C422, C423, C424, C425
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O406, C407, C409, C410, C413
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O416, O421, C417, C418, C419, C420, C422, C423, C424, C425
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O406)=Sof(C407)=Sof(H40A)=Sof(H40B)=Sof(C409)=Sof(H40C)=Sof(H40D)=
 Sof(C410)=Sof(H41A)=Sof(H41B)=Sof(C413)=Sof(H41C)=Sof(H41D)=Sof(O421)=
 Sof(C422)=Sof(H42C)=Sof(H42D)=Sof(C423)=Sof(H42E)=Sof(H42F)=Sof(C424)=
 Sof(H42G)=Sof(H42H)=Sof(C425)=Sof(H42I)=Sof(H42J)=1-FVAR(1)
 Sof(O411)=Sof(C408)=Sof(H40E)=Sof(H40F)=Sof(C412)=Sof(H41E)=Sof(H41F)=
 Sof(C414)=Sof(H41G)=Sof(H41H)=Sof(C415)=Sof(H41I)=Sof(H41J)=Sof(O416)=
 Sof(C417)=Sof(H41K)=Sof(H41L)=Sof(C418)=Sof(H41M)=Sof(H41N)=Sof(C419)=
 Sof(H41O)=Sof(H41P)=Sof(C420)=Sof(H42A)=Sof(H42B)=FVAR(1)
6.a Free rotating group:
 O406(C407,C409,C410,C413), O411(C408,C412,C414,C415), O416(C417,C418,C419,
 C420), O421(C422,C423,C424,C425)
6.b Secondary CH2 refined with riding coordinates:
 C407(H40A,H40B), C409(H40C,H40D), C410(H41A,H41B), C413(H41C,H41D), C408(H40E,
 H40F), C412(H41E,H41F), C414(H41G,H41H), C415(H41I,H41J), C417(H41K,H41L),
 C418(H41M,H41N), C419(H41O,H41P), C420(H42A,H42B), C422(H42C,H42D), C423(H42E,
 H42F), C424(H42G,H42H), C425(H42I,H42J), C402(H40G,H40H), C403(H40I,H40J),
 C404(H40K,H40L), C405(H40M,H40N), C427(H42K,H42L), C428(H42M,H42N), C429(H42O,
 H42P), C430(H43A,H43B)
6.c Idealised Me refined as rotating group:
 C111(H11A,H11B,H11C), C112(H11D,H11E,H11F), C113(H11G,H11H,H11I), C121(H12A,
 H12B,H12C), C122(H12D,H12E,H12F), C123(H12G,H12H,H12I), C131(H13A,H13B,H13C),
 C132(H13D,H13E,H13F), C133(H13G,H13H,H13I), C211(H21A,H21B,H21C), C212(H21D,
 H21E,H21F), C213(H21G,H21H,H21I), C221(H22A,H22B,H22C), C222(H22D,H22E,H22F),
 C223(H22G,H22H,H22I), C232(H23A,H23B,H23C), C233(H23D,H23E,H23F), C234(H23G,
 H23H,H23I), C311(H31A,H31B,H31C), C312(H31D,H31E,H31F), C313(H31G,H31H,H31I),
 C321(H32A,H32B,H32C), C322(H32D,H32E,H32F), C323(H32G,H32H,H32I), C331(H33A,
 H33B,H33C), C332(H33D,H33E,H33F), C333(H33G,H33H,H33I)
;
_shelx_res_checksum              803
_shelx_hkl_checksum              42823
_shelx_fab_checksum              39643
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'