{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_7037999
_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
'C18 H54 Ge9 Si8, 2(C18 H36 K N2 O6), 3(C4 H8 O)'
_chemical_formula_sum            'C66 H150 Ge9 K2 N4 O15 Si8'
_chemical_formula_weight         2196.12
_chemical_properties_physical    'Air-sensitive, Moisture-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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90
_cell_angle_beta                 119.3980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.3009(18)
_cell_length_b                   14.6104(9)
_cell_length_c                   28.7838(17)
_cell_measurement_reflns_used    9780
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.281
_cell_measurement_theta_min      2.565
_cell_volume                     10369.2(11)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_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)'
_diffrn_ambient_temperature      150.02
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0400
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            85281
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.362
_diffrn_reflns_theta_min         1.414
_exptl_absorpt_coefficient_mu    2.794
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0863 before and 0.0362 after correction.
The Ratio of minimum to maximum transmission is 0.7886.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       needle
_exptl_crystal_F_000             4528
_exptl_crystal_size_max          0.341
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.136
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     934
_refine_ls_number_reflns         21134
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0434P)^2^+6.2082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0899
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16228
_reflns_number_total             21134
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04022a2.cif
_cod_data_source_block           k9p21n
_cod_depositor_comments
'Adding full bibliography for 7037998--7038001.cif.'
_cod_database_code               7037999
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C301-C300
 1.6 with sigma of 0.01
 C301-C302
 1.54 with sigma of 0.02
 C310-C311
 1.54 with sigma of 0.02
 C322-C321 = C321-C320 = O320-C320 = O320-C323 = C323-C322
 1.54 with sigma of 0.02
 C123-C122 \\sim C121-C120 \\sim C125-C124
 with sigma of 0.02
3. Others
 Fixed Sof: O320(0.5) C320(0.5) H32A(0.5) H32B(0.5) C321(0.5) H32C(0.5)
 H32D(0.5) O330(0.5) C330(0.5) H33A(0.5) H33B(0.5) C331(0.5) H33C(0.5)
 H33D(0.5) H32E(0.5) H32F(0.5) H32G(0.5) H32H(0.5) H32K(0.5) H32L(0.5)
 H32I(0.5) H32J(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C100(H10J,H10K), C101(H10L,H10M), C102(H10N,H10O), C103(H10P,H10Q), C104(H10R,
 H10S), C105(H10T,H10U), C110(H11J,H11K), C111(H11L,H11M), C112(H11N,H11O),
 C113(H11P,H11Q), C114(H11R,H11S), C115(H11T,H11U), C120(H12J,H12K), C121(H12L,
 H12M), C122(H12N,H12O), C123(H12P,H12Q), C124(H12R,H12S), C125(H12T,H12U),
 C200(H20J,H20K), C201(H20L,H20M), C202(H20N,H20O), C203(H20P,H20Q), C204(H20R,
 H20S), C205(H20T,H20U), C210(H21J,H21K), C211(H21L,H21M), C212(H21N,H21O),
 C213(H21P,H21Q), C214(H21R,H21S), C215(H21T,H21U), C220(H22J,H22K), C221(H22L,
 H22M), C222(H22N,H22O), C223(H22P,H22Q), C224(H22R,H22S), C225(H22T,H22U),
 C300(H30A,H30B), C301(H30C,H30D), C302(H30E,H30F), C303(H30G,H30H), C310(H31A,
 H31B), C311(H31C,H31D), C312(H31E,H31F), C313(H31G,H31H), C320(H32A,H32B),
 C321(H32C,H32D), C330(H33A,H33B), C331(H33C,H33D), C322(H32E,H32F), C322(H32G,
 H32H), C323(H32K,H32L), C323(H32I,H32J)
4.b Me refined with riding coordinates:
 C10A(H10A,H10B,H10C), C10C(H10D,H10E,H10F), C10B(H10G,H10H,H10I), C11A(H11A,
 H11B,H11C), C11C(H11D,H11E,H11F), C11B(H11G,H11H,H11I), C12A(H12A,H12B,H12C),
 C12C(H12D,H12E,H12F), C12B(H12G,H12H,H12I), C20A(H20A,H20B,H20C), C20C(H20D,
 H20E,H20F), C20B(H20G,H20H,H20I), C21B(H21A,H21B,H21C), C21A(H21D,H21E,H21F),
 C21C(H21G,H21H,H21I), C22A(H22A,H22B,H22C), C22C(H22D,H22E,H22F), C22B(H22G,
 H22H,H22I)
;
_shelx_res_checksum              48990
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'