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_1569007
_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         'C48 H65 Ge N3, C3 H7'
_chemical_formula_sum            'C51 H72 Ge N3'
_chemical_formula_weight         799.70
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-07-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
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2022-08-16 deposited with the CCDC.	2023-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                98.596(5)
_cell_angle_beta                 101.664(3)
_cell_angle_gamma                96.759(6)
_cell_formula_units_Z            2
_cell_length_a                   12.7334(7)
_cell_length_b                   13.204(3)
_cell_length_c                   14.3960(6)
_cell_measurement_reflns_used    9822
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      53.87
_cell_measurement_theta_min      2.97
_cell_volume                     2316.3(6)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            37828
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.094
_diffrn_reflns_theta_min         2.980
_diffrn_source_current           3.57
_diffrn_source_power             0.24947159999999996
_diffrn_source_voltage           69.88
_exptl_absorpt_coefficient_mu    0.754
_exptl_absorpt_correction_T_max  0.7532
_exptl_absorpt_correction_T_min  0.6342
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_description       block
_exptl_crystal_F_000             862
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         8363
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+1.9244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1008
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8000
_reflns_number_total             8363
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc07006e2.cif
_cod_data_source_block           LGeMe
_cod_depositor_comments
'Adding full bibliography for 1569006--1569011.cif.'
_cod_original_cell_volume        2316.3(5)
_cod_database_code               1569007
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.902
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C20, C22
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3.a Ternary CH refined with riding coordinates:
 C31(H31), C33(H33), C45(H45), C42(H42)
3.b Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C50(H50A,H50B)
3.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C10(H10), C4(H4), C28(H28), C2(H2), C26(H26), C27(H27), C38(H38),
 C40(H40), C39(H39)
3.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C48(H48A,H48B,H48C), C14(H14A,H14B,H14C), C32(H32A,H32B,
 H32C), C30(H30A,H30B,H30C), C47(H47A,H47B,H47C), C46(H46A,H46B,H46C), C19(H19A,
 H19B,H19C), C35(H35A,H35B,H35C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C),
 C34(H34A,H34B,H34C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C21(H21A,H21B,
 H21C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              57891
_olex2_submission_special_instructions 'No special instructions were received'