A crystalline T-shaped planar group 14 anion.
Liu, Xiaona; Dai, Yuyang; Bao, Manling; Wang, Wenjuan; Li, Qianli; Liu, Chunmeng; Wang, Xinping; Su, Yuanting; Chemical science 14 (2023) 5722–5727; doi:10.1039/d2sc07006e

data_1569010
_publ_section_title
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 A crystalline T-shaped planar group 14 anion.
;
_journal_issue                   21
_journal_name_full               'Chemical science'
_journal_page_first              5722
_journal_page_last               5727
_journal_paper_doi               10.1039/d2sc07006e
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C94 H124 Ge2 K2 N6 S2, 1[C6H14], 2[C4H8O]'
_chemical_formula_sum            'C108 H154 Ge2 K2 N6 O2 S2'
_chemical_formula_weight         1856.020
_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_Int_Tables_number      2
_audit_creation_date             2023-03-21
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2023.03.14 svn.rbb2c1857 for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2023-04-03 deposited with the CCDC.	2023-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                79.781
_cell_angle_beta                 70.505
_cell_angle_gamma                68.035
_cell_formula_units_Z            1
_cell_length_a                   14.1535
_cell_length_b                   14.2181
_cell_length_c                   15.1396
_cell_measurement_reflns_used    7163
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      54.19
_cell_measurement_theta_min      2.93
_cell_volume                     2658.678
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120.00
_diffrn_measured_fraction_theta_full 0.9805
_diffrn_measured_fraction_theta_max 0.9708
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.9805
_diffrn_reflns_Laue_measured_fraction_max 0.9708
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            46015
_diffrn_reflns_point_group_measured_fraction_full 0.9805
_diffrn_reflns_point_group_measured_fraction_max 0.9708
_diffrn_reflns_theta_full        53.5942
_diffrn_reflns_theta_max         54.25
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    1.410
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.6233
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1204 before and 0.0834 after correction.
The Ratio of minimum to maximum transmission is 0.8304.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_description       block
_exptl_crystal_F_000             994.073
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.4847
_refine_diff_density_min         -0.6226
_refine_diff_density_rms         0.0849
_refine_ls_d_res_high            0.8264
_refine_ls_d_res_low             12.5503
_refine_ls_extinction_coef       0.0026(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0354
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    117
_refine_ls_number_parameters     548
_refine_ls_number_reflns         9573
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.0307
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          -0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1404P)^2^+0.7751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1839
_refine_ls_wR_factor_ref         0.2003
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              -15
_reflns_limit_k_max              17
_reflns_limit_k_min              -16
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                7688
_reflns_number_total             9573
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2sc07006e2.cif
_cod_data_source_block           LGeSK
_cod_depositor_comments
'Adding full bibliography for 1569006--1569011.cif.'
_cod_original_cell_volume        2658.677759
_cod_database_code               1569010
_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
 C21A-C20 = C21-C20 = C23A-C20 = C23-C20 = C22A-C20 = C22-C20
 1.54 with sigma of 0.01
 C19A-C16 = C18-C16 = C18A-C16 = C17-C16 = C17A-C16
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C17 \\sim C18 \\sim C19 \\sim C17A \\sim C18A \\sim C19A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 C19A, C16, C18A, C17A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C22A, C20, C23A, C21A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(H17d)=Sof(H17e)=Sof(H17f)=Sof(H19d)=Sof(H19e)=Sof(H19f)=Sof(H18d)=
 Sof(H18e)=Sof(H18f)=Sof(C23)=Sof(H23a)=Sof(H23b)=Sof(C19)=Sof(H23c)=Sof(C21)=
 Sof(H19b)=Sof(H21a)=Sof(H21b)=Sof(H21c)=Sof(H18c)=Sof(H18b)=Sof(H18a)=Sof(C18)=
 Sof(H17b)=Sof(H17c)=Sof(H17a)=Sof(C17)=Sof(H19a)=Sof(C22)=Sof(H22b)=Sof(H22c)=
 Sof(H19c)=Sof(H22a)=1-FVAR(1)
 Sof(H18a)=Sof(H18b)=Sof(H18c)=Sof(H17a)=Sof(H17b)=Sof(H17c)=Sof(H19a)=
 Sof(H19b)=Sof(H19c)=Sof(C23A)=Sof(H17e)=Sof(C17A)=Sof(H23d)=Sof(H23e)=
 Sof(C18A)=Sof(H23f)=Sof(C21A)=Sof(H18e)=Sof(H21d)=Sof(H19d)=Sof(H19f)=
 Sof(C19A)=Sof(H21e)=Sof(H17d)=Sof(H21f)=Sof(H17f)=Sof(C22A)=Sof(H19e)=
 Sof(H22d)=Sof(H18d)=Sof(H22e)=Sof(H18f)=Sof(H22f)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C30(H30), C45(H45), C44(H44), C33(H33)
6.b Me refined with riding coordinates:
 C23A(H23e,H23d,H23f), C21A(H21d,H21f,H21e), C18(H18a,H18b,H18c), C17(H17a,
 H17b,H17c), C19(H19a,H19b,H19c), C17A(H17d,H17e,H17f), C19A(H19d,H19e,H19f),
 C18A(H18d,H18e,H18f)
6.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C40(H40), C2(H2), C4(H4), C28(H28), C39(H39), C8(H8), C27(H27),
 C38(H38), C26(H26)
6.d Idealised Me refined as rotating group:
 C15(H15a,H15b,H15c), C32(H32a,H32b,H32c), C31(H31a,H31b,H31c), C14(H14a,H14b,
 H14c), C47(H47a,H47b,H47c), C46(H46a,H46b,H46c), C42(H42a,H42b,H42c), C23(H23a,
 H23b,H23c), C43(H43a,H43b,H43c), C21(H21a,H21b,H21c), C34(H34a,H34b,H34c),
 C22(H22a,H22b,H22c), C35(H35a,H35b,H35c), C22A(H22d,H22e,H22f)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 141 electrons were 
found in a volume of 675\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 1[C6H14], 2[C4H8O] per Formula Unit 
which account for 130 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'