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_1569009
_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 Se2, 2[C6H14], 2[C4H8O], 2[]'
_chemical_formula_sum            'C114 H168 Ge2 K2 N6 O2 Se2'
_chemical_formula_weight         2035.985
_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
;
2023-04-04 deposited with the CCDC.	2023-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                70.44(2)
_cell_angle_beta                 79.46(2)
_cell_angle_gamma                67.63(2)
_cell_formula_units_Z            1
_cell_length_a                   14.292(8)
_cell_length_b                   14.502(8)
_cell_length_c                   15.149(9)
_cell_measurement_reflns_used    5925
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      53.44
_cell_measurement_theta_min      4.58
_cell_volume                     2730(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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 0.9705
_diffrn_measured_fraction_theta_max 0.9602
_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  0.0553
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.9705
_diffrn_reflns_Laue_measured_fraction_max 0.9602
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37827
_diffrn_reflns_point_group_measured_fraction_full 0.9705
_diffrn_reflns_point_group_measured_fraction_max 0.9602
_diffrn_reflns_theta_full        53.5942
_diffrn_reflns_theta_max         53.98
_diffrn_reflns_theta_min         4.85
_exptl_absorpt_coefficient_mu    1.655
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.6487
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1269 before and 0.0880 after correction.
The Ratio of minimum to maximum transmission is 0.8642.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       block
_exptl_crystal_F_000             1077.416
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
TITL lgesek           P -1         R = 0.07
CELL   14.2920   14.5020   15.1490     70.44     79.46     67.63
SPGR P-1
C101 0.499 0.446 0.096 !       2.13 eA-3
C102 0.497 0.556 0.043 !       2.00 eA-3
C103 0.500 1.000 0.000 !       1.94 eA-3
C104 0.501 0.380 0.052 !       1.69 eA-3
C105 0.154 0.100 0.035 !       1.62 eA-3
C106 0.080 0.109 0.081 !       1.55 eA-3
C107 0.137 0.096 0.111 !       1.37 eA-3
C108 0.184 0.073 0.094 !       1.29 eA-3
C109 0.269 0.111 0.001 !       1.27 eA-3
C110 0.051 0.104 0.166 !       1.25 eA-3
Q111 0.500 1.000 0.500 !       1.15 eA-3
Q112 0.905 0.520 0.187 !       0.87 eA-3
Q113 0.941 0.364 0.136 !       0.85 eA-3
Q114 0.505 0.125 0.377 !       0.81 eA-3
Q115 0.924 0.187 0.104 !       0.70 eA-3
Q116 0.952 0.393 0.224 !       0.68 eA-3
C117 0.863 0.866 0.093 !       0.67 eA-3
Q118 0.885 0.230 0.085 !       0.67 eA-3
Q119 0.833 0.524 0.064 !       0.61 eA-3
Q120 0.155 0.952 0.171 !       0.59 eA-3
Q121 0.497 0.562 0.275 !       0.53 eA-3
Q122 0.483 0.296 0.079 !       0.52 eA-3
Q123 0.904 0.806 0.157 !       0.51 eA-3
Q124 0.282 0.905 0.035 !       0.51 eA-3
Q125 0.858 0.591 0.107 !       0.50 eA-3
Q126 0.491 0.416 0.423 !       0.50 eA-3
;
_refine_diff_density_max         0.9168
_refine_diff_density_min         -0.5202
_refine_diff_density_rms         0.0717
_refine_ls_d_res_high            0.8292
_refine_ls_d_res_low             7.9305
_refine_ls_goodness_of_fit_ref   1.0533
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    118
_refine_ls_number_parameters     559
_refine_ls_number_reflns         9641
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.0501
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          -0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0783P)^2^+2.5037P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1435
_refine_ls_wR_factor_ref         0.1502
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              -16
_reflns_limit_k_max              17
_reflns_limit_k_min              -16
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                8399
_reflns_number_total             9641
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2sc07006e2.cif
_cod_data_source_block           LGeSeK
_cod_depositor_comments
'Adding full bibliography for 1569006--1569011.cif.'
_cod_database_code               1569009
_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
 C20-C21 \\sim C20-C21A
 with sigma of 0.02
 C20-C22 \\sim C20-C22A
 with sigma of 0.02
 C20-C23 \\sim C20-C23A
 with sigma of 0.02
 C3-C16 \\sim C3-C16a
 with sigma of 0.02
 C16-C17 \\sim C16a-C17a
 with sigma of 0.02
 C16-C18 \\sim C16a-C18a
 with sigma of 0.02
 C16-C19 \\sim C16a-C19a
 with sigma of 0.02
 C3-C17 \\sim C3-C17a
 with sigma of 0.04
 C3-C18 \\sim C3-C18a
 with sigma of 0.04
 C3-C19 \\sim C3-C19a
 with sigma of 0.04
 C17-C18 \\sim C17a-C18a
 with sigma of 0.04
 C17-C19 \\sim C17a-C19a
 with sigma of 0.04
 C18-C19 \\sim C18a-C19a
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 C16a, C19a, C17a, C18a, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C21A)=Sof(H21d)=Sof(H21e)=Sof(H21f)=Sof(C22A)=Sof(H22d)=Sof(H22e)=
 Sof(H22f)=Sof(C23A)=Sof(H23d)=Sof(H23e)=Sof(H23f)=1-FVAR(1)
 Sof(C21)=Sof(H21a)=Sof(H21b)=Sof(H21c)=Sof(C22)=Sof(H22a)=Sof(H22b)=Sof(H22c)=
 Sof(C23)=Sof(H23a)=Sof(H23b)=Sof(H23c)=FVAR(1)
 Sof(C16a)=Sof(C17a)=Sof(H17d)=Sof(H17e)=Sof(H17f)=Sof(C18a)=Sof(H18d)=
 Sof(H18e)=Sof(H18f)=Sof(C19a)=Sof(H19d)=Sof(H19e)=Sof(H19f)=Sof(H17d)=
 Sof(H17e)=Sof(H17f)=Sof(H18d)=Sof(H18e)=Sof(H18f)=Sof(H19d)=Sof(H19e)=
 Sof(H19f)=Sof(H17d)=Sof(H17e)=Sof(H17f)=Sof(H18d)=Sof(H18e)=Sof(H18f)=
 Sof(H19d)=Sof(H19e)=Sof(H19f)=Sof(H17d)=Sof(H17e)=Sof(H17f)=Sof(H18d)=
 Sof(H18e)=Sof(H18f)=Sof(H19d)=Sof(H19e)=Sof(H19f)=1-FVAR(2)
 Sof(C16)=Sof(C17)=Sof(H17a)=Sof(H17b)=Sof(H17c)=Sof(C18)=Sof(H18a)=Sof(H18b)=
 Sof(H18c)=Sof(C19)=Sof(H19a)=Sof(H19b)=Sof(H19c)=Sof(H17a)=Sof(H17b)=Sof(H17c)=
 Sof(H18a)=Sof(H18b)=Sof(H18c)=Sof(H19a)=Sof(H19b)=Sof(H19c)=Sof(H17a)=
 Sof(H17b)=Sof(H17c)=Sof(H18a)=Sof(H18b)=Sof(H18c)=Sof(H19a)=Sof(H19b)=
 Sof(H19c)=Sof(H17a)=Sof(H17b)=Sof(H17c)=Sof(H18a)=Sof(H18b)=Sof(H18c)=
 Sof(H19a)=Sof(H19b)=Sof(H19c)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C45(H45), C30(H30), C33(H33), C43(H43)
5.b Me refined with riding coordinates:
 C17(H17a,H17b,H17c), C18(H18a,H18b,H18c), C19(H19a,H19b,H19c), C17a(H17d,H17e,
 H17f), C18a(H18d,H18e,H18f), C19a(H19d,H19e,H19f)
5.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C4(H4), C8(H8), C38(H38), C39(H39), C2(H2), C28(H28), C27(H27),
 C26(H26), C40(H40)
5.d Idealised Me refined as rotating group:
 C15(H15a,H15b,H15c), C14(H14a,H14b,H14c), C47(H47a,H47b,H47c), C32(H32a,H32b,
 H32c), C46(H46a,H46b,H46c), C31(H31a,H31b,H31c), C35(H35a,H35b,H35c), C44(H44a,
 H44b,H44c), C34(H34a,H34b,H34c), C42(H42a,H42b,H42c), C21(H21a,H21b,H21c),
 C22(H22a,H22b,H22c), C23(H23a,H23b,H23c), C21A(H21d,H21e,H21f), C22A(H22d,H22e,
 H22f), C23A(H23d,H23e,H23f)
;
_platon_squeeze_special_details
;
The number of found electrons matches the assignment of 2 hexane and 2 THF molecules, 
which are the solvents used in the crystallisatin of this material.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'