{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_7037998
_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         'C27 H81 Ge9 Si12, C21 H23 K, C7 H8'
_chemical_formula_sum            'C55 H112 Ge9 K Si12'
_chemical_formula_weight         1802.93
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-30
_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                 91.2930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8387(9)
_cell_length_b                   20.2949(13)
_cell_length_c                   27.3283(16)
_cell_measurement_reflns_used    9770
_cell_measurement_temperature    150
_cell_measurement_theta_max      22.991
_cell_measurement_theta_min      2.384
_cell_volume                     8782.3(9)
_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      150.01
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0405
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_laue_measured_fraction_full 0.991
_diffrn_reflns_laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            48652
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        23.301
_diffrn_reflns_theta_max         23.301
_diffrn_reflns_theta_min         1.286
_exptl_absorpt_coefficient_mu    3.274
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1020 before and 0.0413 after correction.
The Ratio of minimum to maximum transmission is 0.6955.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       needle
_exptl_crystal_F_000             3668
_exptl_crystal_size_max          0.335
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.136
_refine_diff_density_max         1.000
_refine_diff_density_min         -0.967
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     725
_refine_ls_number_reflns         12586
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0620
_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^)+(0.0597P)^2^+53.4644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1505
_refine_ls_wR_factor_ref         0.1638
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9218
_reflns_number_total             12586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04022a2.cif
_cod_data_source_block           k1p21c
_cod_depositor_comments
'Adding full bibliography for 7037998--7038001.cif.'
_cod_database_code               7037998
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C201-C200
 1.52 with sigma of 0.02
 Si30-C30A \\sim Si30-C30B \\sim Si30-C30C \\sim Si31-C31A \\sim Si31-C31B
\\sim Si31-C31C
 with sigma of 0.02
 Si32-C32A \\sim Si32-C32B \\sim Si32-C32C \\sim Si33-C33A \\sim Si33-C33B
\\sim Si33-C33C
 with sigma of 0.02
 Si34-C34A \\sim Si34-C34B \\sim Si34-C34C \\sim Si35-C35A \\sim Si35-C35B
\\sim Si35-C35C
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C204 \\sim C203 \\sim C202 \\sim C206 \\sim C201 \\sim C205 \\sim C200: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C204) \\sim Ueq, Uanis(C205) \\sim Ueq, Uanis(C206) \\sim Ueq,
Uanis(C201) \\sim Ueq, Uanis(C202) \\sim Ueq, Uanis(C203) \\sim Ueq,
Uanis(C200) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Fixed Sof: Si3(0.5) Si30(0.5) Si31(0.5) Si32(0.5) Si3A(0.5) Si33(0.5)
 Si34(0.5) Si35(0.5) C10A(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C10B(0.5)
 H10D(0.5) H10E(0.5) H10F(0.5) C10C(0.5) H10G(0.5) H10H(0.5) H10I(0.5)
 C20B(0.5) H20A(0.5) H20B(0.5) H20C(0.5) C20A(0.5) H20D(0.5) H20E(0.5)
 H20F(0.5) C20C(0.5) H20G(0.5) H20H(0.5) H20I(0.5) C30B(0.5) H30A(0.5)
 H30B(0.5) H30C(0.5) C30A(0.5) H30D(0.5) H30E(0.5) H30F(0.5) C30C(0.5)
 H30G(0.5) H30H(0.5) H30I(0.5) C31A(0.5) H31A(0.5) H31B(0.5) H31C(0.5)
 C31B(0.5) H31D(0.5) H31E(0.5) H31F(0.5) C31C(0.5) H31G(0.5) H31H(0.5)
 H31I(0.5) C32C(0.5) H32A(0.5) H32B(0.5) H32C(0.5) C32B(0.5) H32D(0.5)
 H32E(0.5) H32F(0.5) C32A(0.5) H32G(0.5) H32H(0.5) H32I(0.5) C33C(0.5)
 H33A(0.5) H33B(0.5) H33C(0.5) C33B(0.5) H33D(0.5) H33E(0.5) H33F(0.5)
 C33A(0.5) H33G(0.5) H33H(0.5) H33I(0.5) C34B(0.5) H34A(0.5) H34B(0.5)
 H34C(0.5) C34A(0.5) H34D(0.5) H34E(0.5) H34F(0.5) C34C(0.5) H34G(0.5)
 H34H(0.5) H34I(0.5) C35B(0.5) H35A(0.5) H35B(0.5) H35C(0.5) C35A(0.5)
 H35D(0.5) H35E(0.5) H35F(0.5) C35C(0.5) H35G(0.5) H35H(0.5) H35I(0.5)
 C100(0.5) H100(0.5) C102(0.5) H102(0.5) C101(0.5) H101(0.5) C105(0.5)
 H105(0.5) C104(0.5) H104(0.5) C103(0.5) C106(0.5) H10J(0.5) H10K(0.5)
 H10L(0.5) C1AA(0.5) H1AA(0.5) C19(0.5) H19(0.5) C2(0.5) H2(0.5) C2AA(0.5)
 H2AA(0.5) C9(0.5) C5(0.5) H5(0.5) C0AA(0.5) H0AA(0.5) H0AB(0.5) H0AC(0.5)
 C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5) C8(0.5)
 H8A(0.5) H8B(0.5) H8C(0.5) C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C7(0.5) H7A(0.5)
 H7B(0.5) H7C(0.5) C11(0.5) H11J(0.5) H11K(0.5) H11L(0.5)
5.a Ternary CH refined with riding coordinates:
 C112(H112), C111(H111), C110(H110), C121(H121)
5.b Me refined with riding coordinates:
 C10A(H10A,H10B,H10C), C10B(H10D,H10E,H10F), C10C(H10G,H10H,H10I), C11B(H11A,
 H11B,H11C), C11A(H11D,H11E,H11F), C11C(H11G,H11H,H11I), C12B(H12A,H12B,H12C),
 C12A(H12D,H12E,H12F), C12C(H12G,H12H,H12I), C20B(H20A,H20B,H20C), C20A(H20D,
 H20E,H20F), C20C(H20G,H20H,H20I), C21B(H21A,H21B,H21C), C21A(H21D,H21E,H21F),
 C21C(H21G,H21H,H21I), C22C(H22A,H22B,H22C), C22B(H22D,H22E,H22F), C22A(H22G,
 H22H,H22I), C30B(H30A,H30B,H30C), C30A(H30D,H30E,H30F), C30C(H30G,H30H,H30I),
 C31A(H31A,H31B,H31C), C31B(H31D,H31E,H31F), C31C(H31G,H31H,H31I), C32C(H32A,
 H32B,H32C), C32B(H32D,H32E,H32F), C32A(H32G,H32H,H32I), C33C(H33A,H33B,H33C),
 C33B(H33D,H33E,H33F), C33A(H33G,H33H,H33I), C34B(H34A,H34B,H34C), C34A(H34D,
 H34E,H34F), C34C(H34G,H34H,H34I), C35B(H35A,H35B,H35C), C35A(H35D,H35E,H35F),
 C35C(H35G,H35H,H35I), C116(H11M,H11N,H11O), C126(H12J,H12K,H12L), C200(H20J,
 H20K,H20L), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C1(H1A,H1B,H1C),
  C7(H7A,H7B,H7C), C11(H11J,H11K,H11L)
5.c Aromatic/amide H refined with riding coordinates:
 C100(H100), C102(H102), C101(H101), C105(H105), C104(H104), C115(H115),
 C123(H123), C122(H122), C120(H120), C125(H125), C202(H202), C203(H203),
 C204(H204), C205(H205), C206(H206), C1AA(H1AA), C19(H19), C2(H2), C2AA(H2AA),
 C5(H5)
5.d Fitted hexagon refined as free rotating group:
 C100(C102,C101,C105,C104,C103), C114(C113,C112,C111,C110,C115), C124(C123,
 C122,C121,C120,C125), C201(C202,C203,C204,C205,C206), C1AA(C19,C2,C2AA,C9,C5)
5.e Idealised Me refined as rotating group:
 C106(H10J,H10K,H10L), C0AA(H0AA,H0AB,H0AC)
;
_shelx_res_checksum              38940
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'