Observations of tetrel bonding between sp3-carbon and THF
Heywood, Victoria L.; Alford, Thomas P. J.; Roeleveld, Julius J.; Lekanne Deprez, Siebe J.; Verhoofstad, Abraham; van der Vlugt, Jarl Ivar; Domingos, Sérgio R.; Schnell, Melanie; Davis, Anthony P.; Mooibroek, Tiddo J.; Chemical Science 11 (2020) 5289–5293; doi:10.1039/D0SC01559H

data_1558031
_publ_section_title
;
 Observations of tetrel bonding between sp3-carbon and THF
;
_journal_issue                   20
_journal_name_full               'Chemical Science'
_journal_page_first              5289
_journal_page_last               5293
_journal_paper_doi               10.1039/D0SC01559H
_journal_volume                  11
_journal_year                    2020
_chemical_formula_sum            'C13 H14 N4 O'
_chemical_formula_weight         242.28
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-02-11 deposited with the CCDC.	2020-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7490(3)
_cell_length_b                   7.7490(3)
_cell_length_c                   22.0320(11)
_cell_measurement_reflns_used    123
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.8118
_cell_measurement_theta_min      3.8133
_cell_volume                     1322.96(10)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'Bruker ApexII Triumph monochromator sealed tube'
_diffrn_measurement_method       'Photon 50 CMOS detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            63886
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.700
_diffrn_reflns_theta_min         2.786
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.580
_exptl_crystal_size_mid          0.304
_exptl_crystal_size_min          0.244
_exptl_transmission_factor_max   0.7458
_exptl_transmission_factor_min   0.7202
_refine_diff_density_max         0.168
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Flack x determined using 535 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.3(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         1719
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0409
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1171
_reflns_Friedel_coverage         0.595
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1576
_reflns_number_total             1719
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01559h2.cif
_cod_data_source_block           TM_JR_05_THF_0m_a
_cod_depositor_comments
;Adding full bibliography for 1558031.cif.

 Adding full bibliography for 1558031.cif.
;
_cod_original_cell_volume        1322.96(12)
_cod_database_code               1558031
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.954
_shelx_estimated_absorpt_t_max   0.980
_shelx_res_checksum              71125