Symmetry of Three-Center, Four-Electron Bonds
Reiersolmoen, Ann Chrisitn; Battaglia, Stefano; Øien-Ødegaard, Sigurd; Gupta, Arvind Kumar Kumar; Fiksdahl, Anne; Lindh, Roland; Erdelyi, Mate; Chemical Science  (2020) –; doi:10.1039/D0SC02076A

data_1558454
_publ_section_title
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 Symmetry of Three-Center, Four-Electron Bonds
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC02076A
_journal_year                    2020
_chemical_formula_moiety         'C40 H24 N4 Na, C32 H12 B F24'
_chemical_formula_sum            'C72 H36 B F24 N4 Na'
_chemical_formula_weight         1446.85
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-04 deposited with the CCDC.	2020-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.2569(17)
_cell_length_b                   25.817(2)
_cell_length_c                   27.739(3)
_cell_measurement_reflns_used    9774
_cell_measurement_temperature    100
_cell_measurement_theta_max      22.629
_cell_measurement_theta_min      2.429
_cell_volume                     13074(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS, 2016)'
_computing_data_collection       'APEX3 (Bruker AXS, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker Photon100 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture, CMOS detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    'long tubular collimator'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            72074
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        22.804
_diffrn_reflns_theta_max         22.804
_diffrn_reflns_theta_min         2.067
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_T_max  0.7448
_exptl_absorpt_correction_T_min  0.6001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1033 before and 0.0680 after correction. 
The Ratio of minimum to maximum transmission is 0.8057. 
The \l/2 correction factor is Not present.'
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       plate
_exptl_crystal_F_000             5824
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.284
_exptl_crystal_size_min          0.089
_exptl_transmission_factor_max   1.0000
_exptl_transmission_factor_min   0.8057
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     984
_refine_ls_number_reflns         8832
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.1450
_refine_ls_R_factor_gt           0.1096
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+109.3916P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2315
_refine_ls_wR_factor_ref         0.2500
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6451
_reflns_number_total             8832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02076a2.cif
_cod_data_source_block           acr-na-clamp
_cod_database_code               1558454
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.957
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F3AA-C0AA \\sim F0AA-C0AA \\sim F17-C71 \\sim F21-C71 \\sim F24-C71 \\sim
F1AA-C0AA
 with sigma of 0.02
 C71-C44 \\sim C44-C0AA
 with sigma of 0.02
 F4AA-C51 \\sim F5AA-C51 \\sim F6AA-C51 \\sim F20-C51 \\sim F10-C51 \\sim
F22-C51
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F6AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 F3AA, C0AA, F0AA, F1AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F5AA, C51, F6AA, F4AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F1AA)=Sof(F0AA)=Sof(C0AA)=Sof(F3AA)=1-FVAR(1)
 Sof(F17)=Sof(F21)=Sof(F24)=Sof(C71)=FVAR(1)
 Sof(F5AA)=Sof(F4AA)=Sof(F6AA)=1-FVAR(2)
 Sof(F10)=Sof(F20)=Sof(F22)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C7(H7), C8(H8), C9(H9), C14(H14), C17(H17), C18(H18),
 C19(H19), C21(H21), C22(H22), C29(H29), C33(H33), C34(H34), C40(H40), C42(H42),
  C43(H43), C45(H45), C47(H47), C49(H49), C53(H53), C54(H54), C55(H55),
 C57(H57), C58(H58), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C66(H66),
  C67(H67), C68(H68), C69(H69), C70(H70), C72(H72)
;
_shelx_res_checksum              39578
_olex2_submission_special_instructions 'No special instructions were received'