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

data_7712679
_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 Eu4 I4 O20, 4(C27 H81 Ge9 Si12)'
_chemical_formula_sum            'C188 H484 Eu4 Ge36 I4 O20 Si48'
_chemical_formula_weight         8142.72
_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             2021-10-21
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2023-02-13 deposited with the CCDC.	2023-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.3710(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   27.3381(3)
_cell_length_b                   25.0406(3)
_cell_length_c                   29.0012(3)
_cell_measurement_reflns_used    61872
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      24.1210
_cell_measurement_theta_min      2.1320
_cell_volume                     19852.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_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 0.999
_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    -23.00  41.00   0.50   40.00    --  -26.52 -99.00 -60.00  128
  2  \w    -63.00  56.00   0.50   40.00    --  -26.52  37.00 -60.00  238
  3  \w   -140.00 -61.00   0.50   40.00    --  -26.52 178.00  90.00  158
  4  \w     42.00 111.00   0.50   40.00    --   28.39 178.00 120.00  138
  5  \w    -74.00  21.00   0.50   40.00    --   28.39 -37.00 120.00  190
  6  \w     42.00 111.00   0.50   40.00    --   28.39 178.00-180.00  138
  7  \w    -80.00  44.00   0.50   40.00    --   28.39 -57.00-180.00  248
  8  \w     42.00 111.00   0.50   40.00    --   28.39 178.00-150.00  138
  9  \w     42.00 111.00   0.50   40.00    --   28.39 178.00  90.00  138
 10  \w    -86.00 111.00   0.50   40.00    --   28.39   0.00 150.00  394
 11  \w    -28.00  53.00   0.50   40.00    --   28.39  57.00-120.00  162
;
_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      0.0139832000
_diffrn_orient_matrix_UB_12      -0.0231707000
_diffrn_orient_matrix_UB_13      -0.0048111000
_diffrn_orient_matrix_UB_21      0.0218231000
_diffrn_orient_matrix_UB_22      0.0144342000
_diffrn_orient_matrix_UB_23      0.0045494000
_diffrn_orient_matrix_UB_31      -0.0011489000
_diffrn_orient_matrix_UB_32      -0.0075205000
_diffrn_orient_matrix_UB_33      0.0235510000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1342
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            36629
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.750
_diffrn_reflns_theta_max         24.750
_diffrn_reflns_theta_min         2.041
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.790
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.116a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       block
_exptl_crystal_F_000             8120
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: thf'
_exptl_crystal_size_max          0.374
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.067
_refine_diff_density_max         1.297
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1308
_refine_ls_number_reflns         36629
_refine_ls_number_restraints     501
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0696
_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^)+(0.1180P)^2^+4.7392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1704
_refine_ls_wR_factor_ref         0.1836
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26965
_reflns_number_total             36629
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 180.0000\% 
around [1.00 0.00 -0.00] (reciprocal) or [1.00 -0.00 0.01] (direct)
;
_cod_data_source_file            d3dt00578j2.cif
_cod_data_source_block           klementeva_1014_twin1_hklf5_sq
_cod_database_code               7712679
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Eu I O C H Ge Si'
_shelx_estimated_absorpt_t_max   0.785
_shelx_estimated_absorpt_t_min   0.331
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.62604
 0.37396
2. Restrained distances
 I3C-H70J
 2.5 with sigma of 0.02
 H73A-H74B
 2 with sigma of 0.02
 H72C-H72A
 2 with sigma of 0.02
 H74A-H73A
 2 with sigma of 0.02
 H74B-H72O
 2 with sigma of 0.02
 H70A-H71I
 2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
I3A \\sim I3B \\sim I3C: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Eu1A \\sim Eu1B \\sim Eu1C: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O731 \\sim C732 \\sim C733 \\sim C734 \\sim C735: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.04 within 2A
C311 \\sim C312 \\sim C313: within 3A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 3A
Uanis(C737) \\sim Ueq, Uanis(O736) \\sim Ueq, Uanis(C740) \\sim Ueq,
Uanis(C738) \\sim Ueq, Uanis(C739) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C720) \\sim Ueq, Uanis(C719) \\sim Ueq, Uanis(C718) \\sim Ueq,
Uanis(C717) \\sim Ueq, Uanis(O716) \\sim Ueq, Uanis(O721) \\sim Ueq,
Uanis(C722) \\sim Ueq, Uanis(C725) \\sim Ueq, Uanis(C724) \\sim Ueq,
Uanis(C723) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C702) \\sim Ueq, Uanis(C703) \\sim Ueq, Uanis(C750) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(C411) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C531) \\sim Ueq, Uanis(C321) \\sim Ueq, Uanis(C313) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C323) \\sim Ueq, Uanis(C321) \\sim Ueq, Uanis(C322) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 C111, C112, C113, C121, C122, C123, C131, C132, C133, C211, C212, C213, C221,
 C222, C223, C231, C232, C233, C311, C312, C313, C321, C322, C323, C331, C332,
 C333, C411, C412, C413, C421, C422, C423, C431, C432, C433, C511, C512, C513,
 C521, C522, C523, C531, C532, C533, C611, C612, C613, C621, C622, C623, C631,
 C632, C633
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C742, C743, C744, C745
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O701, C702, C703, C704, C705
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O711, C712, C713, C714, C715
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O736, C737, C738, C739, C740
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O746, C747, C748, C749, C750
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O721, C722, C723, C724, C725
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O716, C717, C718, C719, C720
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O706, C707, C708, C709, C710
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O731, C732, C733, C734, C735
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O726, C727, C728, C729, C730
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C411, C412, C413
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Eu1B)=Sof(Eu1C)=0.5*(1-FVAR(2))
 Sof(Eu1A)=FVAR(1)
 Fixed Sof: I1(0.5) I2(0.5) I3A(0.5) I3B(0.25) I3C(0.25)
6.a Free rotating group:
 O701(C702,C703,C704,C705), O706(C707,C708,C709,C710), O711(C712,C713,C714,
 C715), O716(C717,C718,C719,C720), O721(C722,C723,C724,C725), O726(C727,C728,
 C729,C730), O731(C732,C733,C734,C735), O736(C737,C738,C739,C740), O741(C742,
 C743,C744,C745), O746(C747,C748,C749,C750)
6.b Secondary CH2 refined with riding coordinates:
 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), C727(H72K,H72L), C728(H72M,H72N), C729(H72O,
 H72P), C730(H73A,H73B), C732(H73C,H73D), C733(H73E,H73F), C734(H73G,H73H),
 C735(H73I,H73J), C737(H73K,H73L), C738(H73M,H73N), C739(H73O,H73P), C740(H74A,
 H74B), C742(H74C,H74D), C743(H74E,H74F), C744(H74G,H74H), C745(H74I,H74J),
 C747(H74K,H74L), C748(H74M,H74N), C749(H74O,H74P), C750(H75A,H75B)
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(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), 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              27978
_shelx_hkl_checksum              43206
_shelx_fab_checksum              61841
_platon_squeeze_void_probe_radius 1.20
_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 1.308
_oxdiff_exptl_absorpt_empirical_full_min 0.755
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2