Isolation of cationic and neutral (allenylidene)(carbene) and bis(allenylidene)gold complexes
Jin, Liqun; Melaimi, Mohand; Kostenko, Arseni; Karni, Miriam; Apeloig, Yitzhak; Moore, Curtis E.; Rheingold, Arnold L.; Bertrand, Guy; Chem. Sci. 7 (2016) 150–; doi:10.1039/C5SC03654B

data_1540542
_publ_section_title
;
 Isolation of cationic and neutral (allenylidene)(carbene) and
 bis(allenylidene)gold complexes
;
_journal_issue                   1
_journal_name_full               'Chem. Sci.'
_journal_page_first              150
_journal_paper_doi               10.1039/C5SC03654B
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C46 H70 Au N2, B F4, 3(C4 H8 O)'
_chemical_formula_sum            'C58 H94 Au B F4 N2 O3'
_chemical_formula_weight         1151.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-06-03
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-13 deposited with the CCDC.
2015-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                98.507(2)
_cell_angle_beta                 92.5170(19)
_cell_angle_gamma                95.0840(19)
_cell_formula_units_Z            2
_cell_length_a                   12.4983(8)
_cell_length_b                   12.6057(9)
_cell_length_c                   18.1384(12)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.277
_cell_measurement_theta_min      2.205
_cell_volume                     2810.4(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Ultra'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.995
_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       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            52379
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.429
_diffrn_reflns_theta_min         1.137
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.674
_exptl_absorpt_correction_T_max  0.0916
_exptl_absorpt_correction_T_min  0.0674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0889 before and 0.0522 after correction.
The Ratio of minimum to maximum transmission is 0.7358.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_colour_primary    Colorless
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.082
_refine_diff_density_max         1.292
_refine_diff_density_min         -1.659
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.212
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         10333
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.214
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0671
_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^)+(0.0392P)^2^+19.0966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1527
_refine_ls_wR_factor_ref         0.1577
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8908
_reflns_number_total             10333
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03654b2.cif
_cod_data_source_block           MM51
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 1540542--1540544.cif.
;
_cod_database_code               1540542
_shelx_estimated_absorpt_t_max   0.811
_shelx_estimated_absorpt_t_min   0.740
_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. Restrained distances
 C11S-C10S = C12S-C11S
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C3B) = Uanis(Au1B) = Uanis(Au1) = Uanis(C3) = Uanis(C2) = Uanis(C2B)
Uanis(C1) = Uanis(C3) = Uanis(C3B) = Uanis(C1')
4. Rigid body (RIGU) restrains
 O3S, C9S, C10S, C11S, C12S
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(Au1B)=Sof(C2B)=Sof(C3B)=1-FVAR(1)
 Sof(Au1)=Sof(C2)=Sof(C3)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C20(H20), C20'(H20'), C23(H23), C23'(H23')
6.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C6'(H6'A,H6'B), C10(H10C,H10D), C10'(H10A,H10B), C12(H12C,H12D),
 C12'(H12A,H12B), C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,
 H4SB), C5S(H5SA,H5SB), C6S(H6SA,H6SB), C7S(H7SA,H7SB), C8S(H8SA,H8SB),
 C9S(H9SA,H9SB), C10S(H10E,H10F), C11S(H11G,H11H), C12S(H12E,H12F)
6.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C16'(H16'), C17(H17), C17'(H17'), C18(H18), C18'(H18')
6.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C8'(H8'A,H8'B,H8'C), C9(H9A,H9B,H9C), C9'(H9'A,H9'B,H9'C),
 C11(H11D,H11E,H11F), C11'(H11A,H11B,H11C), C13(H13D,H13E,H13F), C13'(H13A,H13B,
 H13C), C21(H21A,H21B,H21C), C21'(H21D,H21E,H21F), C22(H22A,H22B,H22C),
 C22'(H22D,H22E,H22F), C24(H24D,H24E,H24F), C24'(H24A,H24B,H24C), C25(H25D,H25E,
 H25F), C25'(H25A,H25B,H25C)
;
_shelx_res_checksum              43261
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'