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_1569011
_publ_section_title
;
 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         'C59 H86 Ge K N3 O3'
_chemical_formula_sum            'C59 H86 Ge K N3 O3'
_chemical_formula_weight         997.070
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_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                90
_cell_angle_beta                 92.991(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0177(7)
_cell_length_b                   21.7711(13)
_cell_length_c                   24.2953(16)
_cell_measurement_reflns_used    9862
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      53.962
_cell_measurement_theta_min      2.372
_cell_volume                     5819.7(6)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       '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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.00
_diffrn_measured_fraction_theta_full 0.9963
_diffrn_measured_fraction_theta_max 0.9937
_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  0.0847
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 0.9963
_diffrn_reflns_Laue_measured_fraction_max 0.9937
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            79713
_diffrn_reflns_point_group_measured_fraction_full 0.9963
_diffrn_reflns_point_group_measured_fraction_max 0.9937
_diffrn_reflns_theta_full        53.5942
_diffrn_reflns_theta_max         54.00
_diffrn_reflns_theta_min         3.63
_exptl_absorpt_coefficient_mu    1.109
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.5834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1447 before and 0.0954 after correction.
The Ratio of minimum to maximum transmission is 0.7772.
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    1.138
_exptl_crystal_description       block
_exptl_crystal_F_000             2143.530
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.6107
_refine_diff_density_min         -0.5362
_refine_diff_density_rms         0.0747
_refine_ls_d_res_high            0.8290
_refine_ls_d_res_low             10.5970
_refine_ls_goodness_of_fit_ref   1.0263
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    178
_refine_ls_number_parameters     755
_refine_ls_number_reflns         10641
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.0203
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0732P)^2^+3.1388P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1407
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -13
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              -11
_reflns_number_gt                8671
_reflns_number_total             10641
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2sc07006e2.cif
_cod_data_source_block           LGeK
_cod_depositor_comments
'Adding full bibliography for 1569006--1569011.cif.'
_cod_database_code               1569011
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3-C16 \\sim C3-C16a
 with sigma of 0.02
 C16-C19 \\sim C16a-C19a
 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
 C3-C19 \\sim C3-C19a
 with sigma of 0.04
 C3-C17 \\sim C3-C17a
 with sigma of 0.04
 C3-C18 \\sim C3-C18a
 with sigma of 0.04
 C19-C17 \\sim C19a-C17a
 with sigma of 0.04
 C19-C18 \\sim C19a-C18a
 with sigma of 0.04
 C17-C18 \\sim C17a-C18a
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 C16, C18, C19, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C16a, C18a, C19a, C17a
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1A, C48, C49A, C50A, C51A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2, C55A, C54A, C53A, C52A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H42a)=Sof(C43A)=Sof(H43d)=Sof(H43e)=Sof(H43f)=Sof(C44A)=Sof(H44d)=
 Sof(H44e)=Sof(H44f)=Sof(H42a)=Sof(H43d)=Sof(H43e)=Sof(H43f)=Sof(H44d)=
 Sof(H44e)=Sof(H44f)=1-FVAR(1)
 Sof(H42)=Sof(C44)=Sof(H44a)=Sof(H44b)=Sof(H44c)=Sof(C43)=Sof(H43a)=Sof(H43b)=
 Sof(H43c)=Sof(H42)=Sof(H44a)=Sof(H44b)=Sof(H44c)=Sof(H43a)=Sof(H43b)=Sof(H43c)=
 FVAR(1)
 Sof(H48c)=Sof(H48d)=Sof(O1A)=Sof(C51A)=Sof(H51c)=Sof(H51d)=Sof(C50A)=
 Sof(H50c)=Sof(H50d)=Sof(C49A)=Sof(H49c)=Sof(H49d)=Sof(H48c)=Sof(H48d)=
 Sof(H51c)=Sof(H51d)=Sof(H50c)=Sof(H49c)=Sof(H48c)=Sof(H48d)=Sof(H51c)=
 Sof(H50c)=Sof(H49c)=Sof(H48c)=Sof(H48d)=Sof(H51c)=Sof(H51d)=Sof(H50c)=
 Sof(H50d)=Sof(H49c)=Sof(H49d)=1-FVAR(2)
 Sof(O1)=Sof(H48a)=Sof(H48b)=Sof(C49)=Sof(H49a)=Sof(H49b)=Sof(C50)=Sof(H50a)=
 Sof(H50b)=Sof(C51)=Sof(H51a)=Sof(H51b)=Sof(H48a)=Sof(H48b)=Sof(H49a)=Sof(H49b)=
 Sof(H50a)=Sof(H50b)=Sof(H51a)=Sof(H51b)=Sof(H48a)=Sof(H48b)=Sof(H49a)=
 Sof(H49b)=Sof(H50a)=Sof(H50b)=Sof(H51a)=Sof(H51b)=Sof(H48a)=Sof(H48b)=
 Sof(H49a)=Sof(H49b)=Sof(H50a)=Sof(H50b)=Sof(H51a)=Sof(H51b)=FVAR(2)
 Sof(C55A)=Sof(H55c)=Sof(H55d)=Sof(C54A)=Sof(H54c)=Sof(H54d)=Sof(C53A)=
 Sof(H53c)=Sof(H53d)=Sof(C52A)=Sof(H52c)=Sof(H52d)=Sof(H55c)=Sof(H54c)=
 Sof(H54d)=Sof(H53a)=Sof(H53b)=Sof(H52A)=Sof(H55c)=Sof(H55d)=Sof(H54c)=
 Sof(H54d)=Sof(H53c)=Sof(H53d)=Sof(H52c)=Sof(H52d)=1-FVAR(3)
 Sof(C55)=Sof(H55a)=Sof(H55b)=Sof(C52)=Sof(H52a)=Sof(H52b)=Sof(C53)=Sof(H53a)=
 Sof(H53b)=Sof(C54)=Sof(H54a)=Sof(H54b)=Sof(H55a)=Sof(H55b)=Sof(H52)=Sof(H53)=
 Sof(H54a)=Sof(H54b)=Sof(H55a)=Sof(H55b)=Sof(H52a)=Sof(H52b)=Sof(H53a)=
 Sof(H53b)=Sof(H54a)=Sof(H54b)=FVAR(3)
 Sof(C16a)=Sof(C19a)=Sof(H19d)=Sof(H19e)=Sof(H19f)=Sof(C17a)=Sof(H17d)=
 Sof(H17e)=Sof(H17f)=Sof(C18a)=Sof(H18d)=Sof(H18e)=Sof(H18f)=Sof(H19d)=
 Sof(H19e)=Sof(H19f)=Sof(H17d)=Sof(H17e)=Sof(H17f)=Sof(H18d)=Sof(H18e)=
 Sof(H18f)=1-FVAR(4)
 Sof(C16)=Sof(C19)=Sof(H19a)=Sof(H19b)=Sof(H19c)=Sof(C17)=Sof(H17a)=Sof(H17b)=
 Sof(H17c)=Sof(C18)=Sof(H18a)=Sof(H18b)=Sof(H18c)=Sof(H19a)=Sof(H19b)=Sof(H19c)=
 Sof(H17a)=Sof(H17b)=Sof(H17c)=Sof(H18a)=Sof(H18b)=Sof(H18c)=FVAR(4)
5.a Riding coordinates:
 C52A(H52c,H52d)
5.b Ternary CH refined with riding coordinates:
 C33(H33), C30(H30), C45(H45), C42(H42), C42(H42a)
5.c Secondary CH2 refined with riding coordinates:
 C56(H56a,H56b), C59(H59a,H59b), C57(H57a,H57b), C58(H58a,H58b), C55(H55a,
 H55b), C52(H52a,H52b), C53(H53a,H53b), C54(H54a,H54b), C55A(H55c,H55d),
 C54A(H54c,H54d), C53A(H53c,H53d), C48(H48a,H48b), C48(H48c,H48d), C49(H49a,
 H49b), C50(H50a,H50b), C51(H51a,H51b), C51A(H51c,H51d), C50A(H50c,H50d),
 C49A(H49c,H49d)
5.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C8(H8), C4(H4), C2(H2), C28(H28), C27(H27), C26(H26), C40(H40),
 C39(H39), C38(H38)
5.e Idealised Me refined as rotating group:
 C35(H35a,H35b,H35c), C21(H21a,H21b,H21c), C23(H23a,H23b,H23c), C31(H31a,H31b,
 H31c), C34(H34a,H34b,H34c), C32(H32a,H32b,H32c), C15(H15a,H15b,H15c), C14(H14a,
 H14b,H14c), C47(H47a,H47b,H47c), C46(H46a,H46b,H46c), C22(H22a,H22b,H22c),
 C19(H19a,H19b,H19c), C44(H44a,H44b,H44c), C17(H17a,H17b,H17c), C43(H43a,H43b,
 H43c), C18(H18a,H18b,H18c), C43A(H43d,H43e,H43f), C44A(H44d,H44e,H44f),
 C19a(H19d,H19e,H19f), C17a(H17d,H17e,H17f), C18a(H18d,H18e,H18f)
;
_olex2_submission_special_instructions 'No special instructions were received'