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_1558453
_publ_section_title
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 Symmetry of Three-Center, Four-Electron Bonds
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_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC02076A
_journal_year                    2020
_chemical_formula_moiety         '1(C19.84 H12 Au N2), 0.72(C H2 Cl2), B F4'
_chemical_formula_sum            'C20.64 H13.44 Au B Cl1.44 F4 N2'
_chemical_formula_weight         624.28
_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
_audit_creation_date             2020-03-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-17 deposited with the CCDC.	2020-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                85.536(2)
_cell_angle_beta                 86.970(2)
_cell_angle_gamma                78.487(2)
_cell_formula_units_Z            4
_cell_length_a                   6.9430(4)
_cell_length_b                   14.1421(9)
_cell_length_c                   21.3969(14)
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.157
_cell_measurement_theta_min      2.331
_cell_volume                     2050.9(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      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            75183
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.700
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.406
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5433
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1364 before and 0.0549 after correction. 
The Ratio of minimum to maximum transmission is 0.7289. 
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.022
_exptl_crystal_description       prism
_exptl_crystal_F_000             1183
_exptl_crystal_size_max          0.153
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.057
_exptl_transmission_factor_max   1.0000
_exptl_transmission_factor_min   0.7289
_refine_diff_density_max         1.510
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         7250
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0333P)^2^+6.1911P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0850
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5740
_reflns_number_total             7250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02076a2.cif
_cod_data_source_block           acr12-108_soe
_cod_database_code               1558453
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.678
_shelx_estimated_absorpt_t_min   0.397
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C3-C0AA
 1.2 with sigma of 0.02
 C3-N00E
 1.4 with sigma of 0.02
 C1-C00D
 1.4 with sigma of 0.02
 C5-C00G
 1.4 with sigma of 0.02
 C2-C1 = C5-C4
 1.2 with sigma of 0.02
 C9-C1AA
 1.21 with sigma of 0.02
 C1AA-C010 = C9-C00N
 1.4 with sigma of 0.03
 Cl2-C2AA = Cl0A-C2AA
 1.75 with sigma of 0.02
 C3-N00E \\sim C0AA-N00I
 with sigma of 0.02
 C1-C00D \\sim C6-C2
 with sigma of 0.02
 C5-C00G \\sim C4-C00F
 with sigma of 0.02
 C9-C00N \\sim C1AA-C010
 with sigma of 0.01
 Cl2-C2AA \\sim Cl0A-C2AA
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1AA) \\sim Ueq, Uanis(Au11) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2AA) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(B01J) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) = Uanis(C0AA) = Uanis(Au00)
Uanis(C1) = Uanis(Au2) = Uanis(C2)
Uanis(C4) = Uanis(C5) = Uanis(Au1)
4. Rigid body (RIGU) restrains
 Cl2, C2AA, Cl0A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 1*[Sof(Au00)+Sof(C0AA)+Sof(C3)]+1*[Sof(Au1)+Sof(C4)+Sof(C5)]+1*[Sof(Au2)+
 Sof(C1)+Sof(C2)]=1 with esd of 0.001
 Sof(C0AA)=Sof(C3)=1-FVAR(1)
 Sof(Au00)=FVAR(1)
 Sof(C4)=Sof(C5)=1-FVAR(2)
 Sof(Au1)=FVAR(2)
 Sof(C1)=Sof(C2)=1-FVAR(3)
 Sof(Au2)=FVAR(3)
 Sof(Au11)=1-FVAR(4)
 Sof(Au01)=Sof(C1AA)=Sof(C9)=FVAR(4)
 Sof(Cl0A)=Sof(Cl2)=Sof(C2AA)=Sof(H2AA)=Sof(H2AB)=0.5*FVAR(6)
6.a Secondary CH2 refined with riding coordinates:
 C01K(H01B,H01D), C2AA(H2AA,H2AB)
6.b Aromatic/amide H refined with riding coordinates:
 C00O(H00O), C00Q(H00Q), C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V),
 C00W(H00W), C00X(H00X), C00Y(H00Y), C00Z(H00Z), C011(H011), C012(H012),
 C013(H013), C015(H015), C016(H016), C017(H017), C019(H019), C01A(H01A),
 C01C(H01C), C01E(H01E), C01I(H01I), C16(H16), C17(H17), C20(H20)
;
_shelx_res_checksum              87018
_olex2_submission_special_instructions 'No special instructions were received'