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

data_7712681
_publ_section_title
;
 Metalloid germanium cluster shears for lanthanide diiodides
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00578J
_journal_year                    2023
_chemical_formula_moiety
'C80 H160 I4 O20 Sm4, 4(C27 H81 Ge9 Si12), 2(C4 H8 O)'
_chemical_formula_sum            'C196 H500 Ge36 I4 O22 Si48 Sm4'
_chemical_formula_weight         8280.49
_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             2021-06-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-02-13 deposited with the CCDC.	2023-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.138(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   27.108(3)
_cell_length_b                   24.796(2)
_cell_length_c                   28.655(3)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    100
_cell_measurement_theta_max      21.127
_cell_measurement_theta_min      2.172
_cell_volume                     19261(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 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      100
_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  0.1188
_diffrn_reflns_av_unetI/netI     0.0834
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            231890
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.750
_diffrn_reflns_theta_max         24.750
_diffrn_reflns_theta_min         0.711
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    3.866
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1150 before and 0.0763 after correction. The Ratio of minimum to maximum transmission is 0.7891. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       plate
_exptl_crystal_F_000             8272
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: thf'
_exptl_crystal_size_max          0.249
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.056
_refine_diff_density_max         1.588
_refine_diff_density_min         -1.231
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1405
_refine_ls_number_reflns         32967
_refine_ls_number_restraints     346
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0678
_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^)+(0.0541P)^2^+190.8745P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1536
_refine_ls_wR_factor_ref         0.1773
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24302
_reflns_number_total             32967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00578j2.cif
_cod_data_source_block           18_sq
_cod_database_code               7712681
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6317(8)
 0.3683(8)
2. 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
3. Restrained distances
 H70H-H71J
 2 with sigma of 0.02
 H70J-H72B
 2 with sigma of 0.02
 H73C-H70E
 2.1 with sigma of 0.02
 C742-C743 = O741-C745 = C744-C745 = C744-C743
 1.54 with sigma of 0.02
 C753-C752 = C754-C753 = C754-C755
 1.54 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O746 \\sim C747 \\sim C748 \\sim C749 \\sim C750: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
O726 \\sim C727 \\sim C728 \\sim C729 \\sim C730: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
O736 \\sim C737 \\sim C738 \\sim C739 \\sim C740: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
O701 \\sim C702 \\sim C703 \\sim C704 \\sim C705: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
O711 \\sim C712 \\sim C713 \\sim C714 \\sim C715: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
O706 \\sim C707 \\sim C708 \\sim C709 \\sim C710: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
O716 \\sim C717 \\sim C718 \\sim C719 \\sim C720: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
O721 \\sim C722 \\sim C723 \\sim C724 \\sim C725: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
I3A \\sim I3B \\sim I3C: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Sm1A \\sim Sm1B \\sim Sm1C: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Sm2A \\sim Sm2B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(I3C) \\sim Ueq, Uanis(I3B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C131) \\sim Ueq, Uanis(C141) \\sim Ueq, Uanis(C133) \\sim Ueq,
Uanis(C142) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C111) \\sim Ueq, Uanis(C113) \\sim Ueq, Uanis(C112) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(I3C) = Uanis(I3B)
Uanis(Sm1C) = Uanis(Sm1B)
5. Others
 Sof(Sm1C)=Sof(I3C)=0.5*(1-FVAR(2))
 Sof(Sm1B)=Sof(I3B)=0.5*FVAR(2)
 Sof(Si14)=Sof(H13G)=Sof(H13H)=Sof(H13I)=Sof(C141)=Sof(H14A)=Sof(H14B)=
 Sof(H14C)=Sof(C142)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(2)
 Sof(Si13)=Sof(C131)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(H13D)=Sof(H13E)=
 Sof(H13F)=Sof(C133)=Sof(H13J)=Sof(H13K)=Sof(H13L)=FVAR(2)
 Fixed Sof: Sm1A(0.5) I1(0.5) Sm2A(0.5) Sm2B(0.5) I2(0.5) I3A(0.5)
6.a Free rotating group:
 O726(C727,C728,C729,C730), O736(C737,C738,C739,C740), O746(C747,C748,C749,
 C750), O701(C702,C703,C704,C705), O706(C707,C708,C709,C710), O711(C712,C713,
 C714,C715), O716(C717,C718,C719,C720)
6.b Secondary CH2 refined with riding coordinates:
 C727(H72K,H72L), C728(H72M,H72N), C729(H72O,H72P), C730(H73A,H73B), C737(H1,
 H737), C738(H73C,H73D), C739(H73E,H73F), C740(H74A,H74B), C747(H74C,H74D),
 C748(H74E,H74F), C749(H74G,H74H), C750(H75A,H75B), C732(H73G,H73H), C733(H73I,
 H73J), C734(H73K,H73L), C735(H73M,H73N), C742(H74I,H74J), C743(H74K,H74L),
 C744(H74M,H74N), C745(H74O,H74P), C702(H70A,H70B), C703(H70C,H70D), C704(H70E,
 H70F), C705(H70G,H70H), C707(H70I,H70J), C708(H70K,H70L), C709(H70M,H70N),
 C710(H71A,H71B), C712(H71C,H71D), C713(H71E,H71F), C714(H71G,H71H), C715(H71I,
 H71J), C717(H71K,H71L), C718(H71M,H71N), C719(H71O,H71P), C720(H72A,H72B),
 C722(H72C,H72D), C723(H72E,H72F), C724(H72G,H72H), C725(H72I,H72J), C752(H75C,
 H75D), C753(H75E,H75F), C754(H75G,H75H), C755(H75I,H75J)
6.c Me refined with riding coordinates:
 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(H13G,H13H,H13I), C132(H13D,H13E,H13F), C133(H13J,H13K,H13L), C141(H14A,
 H14B,H14C), C142(H14D,H14E,H14F), C211(H21A,H21B,H21C), C212(H21D,H21E,H21F),
 C213(H21G,H21H,H21I), C221(H22A,H22B,H22C), C222(H22D,H22E,H22F), C223(H22G,
 H22H,H22I), C231(H23A,H23B,H23C), C232(H23D,H23E,H23F), C233(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), C411(H41A,H41B,H41C), C412(H41D,
 H41E,H41F), C413(H41G,H41H,H41I), C421(H42A,H42B,H42C), C422(H42D,H42E,H42F),
 C423(H42G,H42H,H42I), C431(H43A,H43B,H43C), C432(H43D,H43E,H43F), C433(H43G,
 H43H,H43I), C511(H51A,H51B,H51C), C512(H51D,H51E,H51F), C513(H51G,H51H,H51I),
 C521(H52A,H52B,H52C), C522(H52D,H52E,H52F), C523(H52G,H52H,H52I), C531(H53A,
 H53B,H53C), C532(H53D,H53E,H53F), C533(H53G,H53H,H53I), C611(H61A,H61B,H61C),
 C612(H61D,H61E,H61F), C613(H61G,H61H,H61I), C621(H62A,H62B,H62C), C622(H62D,
 H62E,H62F), C623(H62G,H62H,H62I), C631(H63A,H63B,H63C), C632(H63D,H63E,H63F),
 C633(H63G,H63H,H63I)
;
_shelx_res_checksum              96680
_shelx_hkl_checksum              30241
_shelx_fab_checksum              22209
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'