{Ge9[Si(SiMe3)3]2}(2-): a starting point for mixed substituted metalloid germanium clusters.
Kysliak, O.; Schnepf, A.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 2404–2408; doi:10.1039/c5dt04022a

data_7038000
_publ_section_title
;
 {Ge9[Si(SiMe3)3]2}(2-): a starting point for mixed substituted metalloid
 germanium clusters.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2404
_journal_page_last               2408
_journal_paper_doi               10.1039/c5dt04022a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C54 H111 Ge9 K O3 Si12'
_chemical_formula_sum            'C54 H111 Ge9 K O3 Si12'
_chemical_formula_weight         1837.91
_chemical_name_systematic
;
 ? 
;
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-01
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-12-01 deposited with the CCDC.
2015-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                97.312(2)
_cell_angle_beta                 94.153(2)
_cell_angle_gamma                108.939(2)
_cell_formula_units_Z            2
_cell_length_a                   12.1599(11)
_cell_length_b                   15.0580(14)
_cell_length_c                   27.802(3)
_cell_measurement_reflns_used    6416
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.458
_cell_measurement_theta_min      2.389
_cell_volume                     4740.7(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v.2014.1-1 (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0844
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            39721
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.406
_diffrn_reflns_theta_min         1.448
_exptl_absorpt_coefficient_mu    3.037
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1097 before and 0.0434 after correction.
The Ratio of minimum to maximum transmission is 0.7921.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1868
_exptl_crystal_size_max          0.413
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.865
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         19284
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0433P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.1031
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12225
_reflns_number_total             19284
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04022a2.cif
_cod_data_source_block           k30p-1
_cod_depositor_comments
'Adding full bibliography for 7037998--7038001.cif.'
_cod_database_code               7038000
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C122-C121 = C123-C122 = C132-C131 = C133-C132 = C131-C130 = C121-C120
 1.54 with sigma of 0.02
3. Others
 Fixed Sof: C10A(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C10C(0.5) H10D(0.5)
 H10E(0.5) H10F(0.5) C10B(0.5) H10G(0.5) H10H(0.5) H10I(0.5) C30C(0.5)
 H30A(0.5) H30B(0.5) H30C(0.5) C30B(0.5) H30D(0.5) H30E(0.5) H30F(0.5)
 C30A(0.5) H30G(0.5) H30H(0.5) H30I(0.5) C30F(0.5) H30J(0.5) H30K(0.5)
 H30L(0.5) C30E(0.5) H30M(0.5) H30N(0.5) H30O(0.5) C30D(0.5) H30P(0.5)
 H30Q(0.5) H30R(0.5) O110(0.5) C110(0.5) H11J(0.5) H11K(0.5) C111(0.5)
 H11L(0.5) H11M(0.5) C112(0.5) H11N(0.5) H11O(0.5) C113(0.5) H11P(0.5)
 H11Q(0.5) C120(0.5) H12J(0.5) H12K(0.5) C121(0.5) H12L(0.5) H12M(0.5)
 C122(0.5) H12N(0.5) H12O(0.5) C123(0.5) H12P(0.5) H12Q(0.5) C130(0.5)
 H13A(0.5) H13B(0.5) C131(0.5) H13C(0.5) H13D(0.5) C132(0.5) H13E(0.5)
 H13F(0.5) C133(0.5) H13G(0.5) H13H(0.5) C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5)
 C0AA(0.5) H0AA(0.5) H0AB(0.5) H0AC(0.5) C1AA(0.5) H1AA(0.5) H1AB(0.5)
 H1AC(0.5) O121(0.5) C3(0.5) H3A(0.5) H3B(0.5) C4(0.5) H4A(0.5) H4B(0.5)
 C5(0.5) H5A(0.5) H5B(0.5) C7(0.5) H7A(0.5) H7B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C100(H10J,H10K), C101(H10L,H10M), C102(H10N,H10O), C103(H10P,H10Q), C110(H11J,
 H11K), C111(H11L,H11M), C112(H11N,H11O), C113(H11P,H11Q), C120(H12J,H12K),
 C121(H12L,H12M), C122(H12N,H12O), C123(H12P,H12Q), C130(H13A,H13B), C131(H13C,
 H13D), C132(H13E,H13F), C133(H13G,H13H), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B),
  C7(H7A,H7B)
4.b Me refined with riding coordinates:
 C10A(H10A,H10B,H10C), C10C(H10D,H10E,H10F), C10B(H10G,H10H,H10I), C1(H1A,H1B,
 H1C), C0AA(H0AA,H0AB,H0AC), C1AA(H1AA,H1AB,H1AC)
4.c Aromatic/amide H refined with riding coordinates:
 C22H(H22H), C22N(H22N), C22F(H22F), C22R(H22R), C22Q(H22Q), C22P(H22P),
 C22O(H22O), C22L(H22L), C22B(H22B), C22E(H22E), C22K(H22K), C22I(H22I),
 C22D(H22D), C22J(H22J), C22C(H22C)
4.d Idealised Me refined as rotating group:
 C11C(H11A,H11B,H11C), C11B(H11D,H11E,H11F), C11A(H11G,H11H,H11I), C12B(H12A,
 H12B,H12C), C12A(H12D,H12E,H12F), C12C(H12G,H12H,H12I), C20C(H20A,H20B,H20C),
 C20B(H20D,H20E,H20F), C20A(H20G,H20H,H20I), C21C(H21A,H21B,H21C), C21B(H21D,
 H21E,H21F), C21A(H21G,H21H,H21I), C30C(H30A,H30B,H30C), C30B(H30D,H30E,H30F),
 C30A(H30G,H30H,H30I), C30F(H30J,H30K,H30L), C30E(H30M,H30N,H30O), C30D(H30P,
 H30Q,H30R), C31C(H31A,H31B,H31C), C31B(H31D,H31E,H31F), C31A(H31G,H31H,H31I),
 C32C(H32A,H32B,H32C), C32B(H32D,H32E,H32F), C32A(H32G,H32H,H32I)
;
_shelx_res_checksum              16745
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'