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_1569008
_publ_section_title
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 A crystalline T-shaped planar group 14 anion.
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_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 Li6 N6, 2.38[C6H14]'
_chemical_formula_sum            'C108.28 H157.32 Li6 N6'
_chemical_formula_weight         1584.71
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-01
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
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2023-04-03 deposited with the CCDC.	2023-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.595(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4571(7)
_cell_length_b                   42.796(2)
_cell_length_c                   15.4362(9)
_cell_measurement_reflns_used    9804
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      53.24
_cell_measurement_theta_min      2.65
_cell_volume                     9519.8(8)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0861
_diffrn_reflns_av_unetI/netI     0.0676
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            103054
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.013
_diffrn_reflns_theta_min         2.815
_diffrn_source_current           3.57
_diffrn_source_power             0.24947159999999996
_diffrn_source_voltage           69.88
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_description       block
_exptl_crystal_F_000             3468
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1017
_refine_ls_number_reflns         17456
_refine_ls_number_restraints     566
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0639
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1041P)^2^+2.1874P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1761
_refine_ls_wR_factor_ref         0.1958
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11597
_reflns_number_total             17456
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc07006e2.cif
_cod_data_source_block           L2Li6
_cod_depositor_comments
'Adding full bibliography for 1569006--1569011.cif.'
_cod_original_cell_volume        9519.8(9)
_cod_database_code               1569008
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.971
_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. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3.a Ternary CH refined with riding coordinates:
 C30(H30), C33(H33), C45(H45), C80(H80), C89(H89), C92(H92)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C8(H8), C10(H10), C26(H26), C27(H27), C28(H28), C38(H38),
 C39(H39), C40(H40), C49(H49), C51(H51), C57(H57), C59(H59), C73(H73), C74(H74),
  C75(H75), C85(H85), C86(H86), C87(H87)
3.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), C46(H46A,H46B,H46C), C47(H47A,H47B,
 H47C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C65(H65A,
 H65B,H65C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C),
 C70(H70A,H70B,H70C), C78(H78A,H78B,H78C), C81(H81A,H81B,H81C), C82(H82A,H82B,
 H82C), C90(H90A,H90B,H90C), C91(H91A,H91B,H91C), C93(H93A,H93B,H93C), C94(H94A,
 H94B,H94C)
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_smtbx_masks_special_details
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A solvent mask was calculated and 476 electrons were 
found in a volume of 2280\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2.38[C6H14] per Asymmetric Unit 
which account for 476 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              10501
_shelx_fab_checksum              95859
_olex2_submission_special_instructions 'No special instructions were received'