(thf)<sub>2</sub>Ln(Ge<sub>9</sub>{Si(SiMe<sub>3</sub>)<sub>3</sub>}<sub>3</sub>)<sub>2</sub> (Ln = Eu, Sm): the first coordination of metalloid germanium clusters to lanthanides.
Klementyeva, Svetlana V.; Schrenk, Claudio; Zhang, Minghui; Khusniyarov, Marat M.; Schnepf, Andreas; Chemical communications (Cambridge, England) 57 (2021) 4730–4733; doi:10.1039/d1cc01151k

data_7128123
_publ_section_title
;
 (thf)<sub>2</sub>Ln(Ge<sub>9</sub>{Si(SiMe<sub>3</sub>)<sub>3</sub>}<sub>3</sub>)<sub>2</sub>
 (Ln = Eu, Sm): the first coordination of metalloid germanium clusters to
 lanthanides.
;
_journal_issue                   38
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4730
_journal_page_last               4733
_journal_paper_doi               10.1039/d1cc01151k
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C62 H178 Ge18 O2 Si24 Sm, 2(C6 H14)'
_chemical_formula_sum            'C74 H206 Ge18 O2 Si24 Sm'
_chemical_formula_weight         3259.51
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-10 deposited with the CCDC.	2021-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.337(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.788(5)
_cell_length_b                   24.181(5)
_cell_length_c                   29.737(6)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    150
_cell_measurement_theta_max      21.114
_cell_measurement_theta_min      2.204
_cell_volume                     15157(6)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 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      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 0.995
_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  0.1136
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            250840
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.491
_diffrn_reflns_theta_min         1.283
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    4.110
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5298
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1408 before and 0.0564 after correction. The Ratio of minimum to maximum transmission is 0.7108. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'light orange'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       irregular
_exptl_crystal_F_000             6560
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: thf, hexane'
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.038
_refine_diff_density_max         1.134
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1183
_refine_ls_number_reflns         31226
_refine_ls_number_restraints     363
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0455P)^2^+36.9081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1262
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19279
_reflns_number_total             31226
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01151k2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7128123--7128124.cif.'
_cod_original_cell_volume        15157(5)
_cod_database_code               7128123
_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
 C818-C817 = C817-C816 = C816-C815 = C815-C814 = C814-C813
 1.54 with sigma of 0.02
 C801-C802 \\sim C802-C803 \\sim C803-C804 \\sim C804-C805 \\sim C805-C806
 with sigma of 0.02
 C801-C803 \\sim C803-C805 \\sim C802-C804 \\sim C804-C806
 with sigma of 0.04
 C807-C808 \\sim C808-C809 \\sim C809-C810 \\sim C810-C811 \\sim C811-C812
 with sigma of 0.02
 C807-C809 \\sim C809-C811 \\sim C808-C810 \\sim C810-C812
 with sigma of 0.04
 C802-C801 \\sim C803-C802 \\sim C804-C803 \\sim C805-C804 \\sim C806-C805
\\sim C808-C807 \\sim C809-
 C808 \\sim C809-C810 \\sim C811-C810 \\sim C812-C811
 with sigma of 0.02
 C813-C814 \\sim C814-C815 \\sim C815-C816 \\sim C816-C817 \\sim C817-C818
 with sigma of 0.02
 C813-C815 \\sim C815-C817 \\sim C814-C816 \\sim C816-C818
 with sigma of 0.04
 C818-C816 \\sim C817-C815 \\sim C816-C814 \\sim C815-C813
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C801 \\sim C802 \\sim C803 \\sim C804 \\sim C805 \\sim C806: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C807 \\sim C808 \\sim C809 \\sim C810 \\sim C811 \\sim C812: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C813 \\sim C814 \\sim C815 \\sim C816 \\sim C817 \\sim C818: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C812 \\sim C818: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C811 \\sim C817: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C810 \\sim C816: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C809 \\sim C815: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C808 \\sim C814: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C807 \\sim C813: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C812) \\sim Ueq, Uanis(C811) \\sim Ueq, Uanis(C810) \\sim Ueq,
Uanis(C809) \\sim Ueq, Uanis(C808) \\sim Ueq, Uanis(C807) \\sim Ueq: with sigma
of 0.03 and sigma for terminal atoms of 0.06
Uanis(C814) \\sim Ueq, Uanis(C813) \\sim Ueq, Uanis(C815) \\sim Ueq,
Uanis(C817) \\sim Ueq, Uanis(C816) \\sim Ueq, Uanis(C818) \\sim Ueq: with sigma
of 0.03 and sigma for terminal atoms of 0.06
4. Rigid body (RIGU) restrains
 C801, C802, C803, C804, C805, C806
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C807, C808, C809, C810, C811, C812
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C813, C814, C815, C816, C817, C818
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C813)=Sof(H81H)=Sof(H81I)=Sof(H81J)=Sof(C814)=Sof(H81K)=Sof(H81L)=
 Sof(C815)=Sof(H81M)=Sof(H81N)=Sof(C816)=Sof(H81O)=Sof(H81P)=Sof(C817)=
 Sof(H81Q)=Sof(H81R)=Sof(C818)=Sof(H81S)=Sof(H81T)=Sof(H81U)=1-FVAR(1)
 Sof(C807)=Sof(H80O)=Sof(H80P)=Sof(H80Q)=Sof(C808)=Sof(H80R)=Sof(H80S)=
 Sof(C809)=Sof(H80T)=Sof(H80U)=Sof(C810)=Sof(H81A)=Sof(H81B)=Sof(C811)=
 Sof(H81C)=Sof(H81D)=Sof(C812)=Sof(H81E)=Sof(H81F)=Sof(H81G)=FVAR(1)
6.a 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), C802(H80D,H80E),
 C803(H80F,H80G), C804(H80H,H80I), C805(H80J,H80K), C808(H80R,H80S), C809(H80T,
 H80U), C810(H81A,H81B), C811(H81C,H81D), C814(H81K,H81L), C815(H81M,H81N),
 C816(H81O,H81P), C817(H81Q,H81R)
6.b Me refined with riding coordinates:
 C807(H80O,H80P,H80Q), C812(H81E,H81F,H81G), C813(H81H,H81I,H81J), C818(H81S,
 H81T,H81U)
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), 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), C801(H80A,H80B,H80C), C806(H80L,H80M,H80N)
;
_shelx_res_checksum              40561
_olex2_submission_special_instructions 'No special instructions were received'