{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_7038001
_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         'C39 H105 Ge9 K O3 Si12, C5 H7'
_chemical_formula_sum            'C44 H117 Ge9 K O3 Si12'
_chemical_formula_weight         1723.86
_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             2015-12-01
_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                 112.221(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.448(4)
_cell_length_b                   11.2469(18)
_cell_length_c                   30.221(4)
_cell_measurement_reflns_used    4943
_cell_measurement_temperature    150
_cell_measurement_theta_max      22.355
_cell_measurement_theta_min      2.322
_cell_volume                     8322(2)
_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
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART Apex'
_diffrn_measurement_method       'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_unetI/netI     0.1044
_diffrn_reflns_laue_measured_fraction_full 0.994
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            30163
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        23.210
_diffrn_reflns_theta_max         23.210
_diffrn_reflns_theta_min         1.377
_exptl_absorpt_coefficient_mu    3.454
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.5166
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0771 before and 0.0422 after correction.
The Ratio of minimum to maximum transmission is 0.6935.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       needle
_exptl_crystal_F_000             3520
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         11828
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1146
_refine_ls_R_factor_gt           0.0562
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0606P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1339
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7249
_reflns_number_total             11828
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04022a2.cif
_cod_data_source_block           mo_kysliak_20_0m
_cod_depositor_comments
'Adding full bibliography for 7037998--7038001.cif.'
_cod_database_code               7038001
_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
 C201-C202
 1.54 with sigma of 0.02
 C202-C203
 1.54 with sigma of 0.02
 C203-C204
 1.54 with sigma of 0.02
 C204-C205
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C111 \\sim C112 \\sim C110 \\sim C109: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4.a Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B), C102(H10C,H10D), C103(H10E,H10F), C104(H10G,H10H), C105(H10I,
 H10J), C106(H10K,H10L), C107(H10M,H10N), C108(H10O,H10P), C109(H10Q,H10R),
 C110(H11D,H11E), C111(H11F,H11G), C112(H11H,H11I), C202(H20A,H20B), C204(H20C,
 H20D)
4.b Me refined with riding coordinates:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,
 H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C),
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,
 H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C),
 C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C205(H20E,H20F,H20G)
;
_shelx_res_checksum              20739
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'