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_1569006
_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         'C47 H62 Cl2 Ge N3'
_chemical_formula_sum            'C47 H62 Cl2 Ge N3'
_chemical_formula_weight         812.554
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_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
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2023-04-04 deposited with the CCDC.	2023-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.550(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.6991(18)
_cell_length_b                   18.5153(9)
_cell_length_c                   15.1604(8)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.927
_cell_measurement_theta_min      2.521
_cell_volume                     8869.9(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      120.06
_diffrn_measured_fraction_theta_full 0.9970
_diffrn_measured_fraction_theta_max 0.9973
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.9970
_diffrn_reflns_Laue_measured_fraction_max 0.9973
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            50335
_diffrn_reflns_point_group_measured_fraction_full 0.9970
_diffrn_reflns_point_group_measured_fraction_max 0.9973
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    0.846
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1471 before and 0.0708 after correction. The Ratio of minimum to maximum transmission is 0.6100. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light purple'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    purple
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       block
_exptl_crystal_F_000             3453.726
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.4058
_refine_diff_density_min         -0.3291
_refine_diff_density_rms         0.0578
_refine_ls_d_res_high            0.8107
_refine_ls_d_res_low             7.9875
_refine_ls_extinction_coef       0.00103(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0575
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    118
_refine_ls_number_parameters     650
_refine_ls_number_reflns         8708
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      1.0490
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          -0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+9.4252P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1172
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              38
_reflns_limit_h_min              -39
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                7252
_reflns_number_total             8708
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2sc07006e2.cif
_cod_data_source_block           LGeCl2
_cod_depositor_comments
'Adding full bibliography for 1569006--1569011.cif.'
_cod_database_code               1569006
_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
 C9-C20 \\sim C9-C20A
 with sigma of 0.02
 C20-C21 \\sim C20A-C21A
 with sigma of 0.02
 C20-C22 \\sim C20A-C22A
 with sigma of 0.02
 C20-C23 \\sim C20A-C23A
 with sigma of 0.02
 C9-C21 \\sim C9-C21A
 with sigma of 0.04
 C9-C22 \\sim C9-C22A
 with sigma of 0.04
 C9-C23 \\sim C9-C23A
 with sigma of 0.04
 C21-C22 \\sim C21A-C22A
 with sigma of 0.04
 C21-C23 \\sim C21A-C23A
 with sigma of 0.04
 C22-C23 \\sim C22A-C23A
 with sigma of 0.04
 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
 C20, C22, C21, C23, C9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3, C18A, C16A, C19A, C17A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C9, C20A, C21A, C23A, C22A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C20A)=Sof(C21A)=Sof(H21d)=Sof(H21e)=Sof(H21f)=Sof(C22A)=Sof(H22d)=
 Sof(H22e)=Sof(H22f)=Sof(C23A)=Sof(H23d)=Sof(H23e)=Sof(H23f)=Sof(H21d)=
 Sof(H21e)=Sof(H21f)=Sof(H22d)=Sof(H22e)=Sof(H22f)=Sof(H23d)=Sof(H23e)=
 Sof(H23f)=1-FVAR(1)
 Sof(C20)=Sof(C21)=Sof(H21a)=Sof(H21b)=Sof(H21c)=Sof(C22)=Sof(H22a)=Sof(H22b)=
 Sof(H22c)=Sof(C23)=Sof(H23a)=Sof(H23b)=Sof(H23c)=Sof(H21a)=Sof(H21b)=Sof(H21c)=
 Sof(H22a)=Sof(H22b)=Sof(H22c)=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)=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)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C30(H30), C33(H33), C42(H42), C45(H45)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C2(H2), C8(H8), C10(H10), C28(H28), C27(H27), C26(H26), C40(H40),
 C39(H39), C38(H38)
5.c Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C15(H15a,H15b,H15c), C17(H17a,H17b,H17c), C18(H18a,H18b,
 H18c), C19(H19a,H19b,H19c), C21(H21a,H21b,H21c), C22(H22a,H22b,H22c), C23(H23a,
 H23b,H23c), C31(H31a,H31b,H31c), C32(H32a,H32b,H32c), C34(H34a,H34b,H34c),
 C35(H35a,H35b,H35c), C43(H43a,H43b,H43c), C44(H44a,H44b,H44c), C46(H46a,H46b,
 H46c), C47(H47a,H47b,H47c), C21A(H21d,H21e,H21f), C22A(H22d,H22e,H22f),
 C23A(H23d,H23e,H23f), C17A(H17d,H17e,H17f), C18A(H18d,H18e,H18f), C19A(H19d,
 H19e,H19f)
;
_olex2_submission_special_instructions 'No special instructions were received'