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_1540544
_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         'C48 H70 Au N2, B F4, 2(C H2 Cl2)'
_chemical_formula_sum            'C50 H74 Au B Cl4 F4 N2'
_chemical_formula_weight         1128.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 106.993(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.393(4)
_cell_length_b                   14.569(4)
_cell_length_c                   24.605(6)
_cell_measurement_reflns_used    4025
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.933
_cell_measurement_theta_min      2.338
_cell_volume                     5277(2)
_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  'ShelXL (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 0.996
_diffrn_measured_fraction_theta_max 0.989
_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  0.0732
_diffrn_reflns_av_unetI/netI     0.0947
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            28966
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.448
_diffrn_reflns_theta_min         1.731
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.039
_exptl_absorpt_correction_T_max  0.0627
_exptl_absorpt_correction_T_min  0.0315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0863 before and 0.0431 after correction.
The Ratio of minimum to maximum transmission is 0.5024.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.147
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.054
_refine_diff_density_max         1.426
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         10760
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1203
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0468P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1179
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5731
_reflns_number_total             10760
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03654b2.cif
_cod_data_source_block           MM50
_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.

'_exptl_crystal_colour_primary' value 'Yellow' changed to 'yellow'
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               1540544
_shelx_estimated_absorpt_t_max   0.853
_shelx_estimated_absorpt_t_min   0.664
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1S-C1S = Cl2S-C1S = Cl2B-C1SB = Cl1B-C1SB
 1.8 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C1SB) = Uanis(C1S)
Uanis(Cl1S) = Uanis(Cl1B)
Uanis(Cl2S) = Uanis(Cl2B)
Uanis(F2B) = Uanis(F2)
Uanis(F4B) = Uanis(F4)
Uanis(F1) = Uanis(F1B)
Uanis(F3) = Uanis(F3B)
4. Rigid body (RIGU) restrains
 F1, F2, F3, F4, F1B, F2B, F3B, F4B, B1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1S, Cl2S, Cl1B, Cl2B, C1S, C1SB
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Cl3S, Cl4S, Cl3B, Cl4B, C2S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Cl3B)=Sof(Cl4B)=Sof(H2SC)=Sof(H2SD)=1-FVAR(1)
 Sof(Cl3S)=Sof(Cl4S)=Sof(H2SA)=Sof(H2SB)=FVAR(1)
 Sof(Cl1B)=Sof(Cl2B)=Sof(C1SB)=Sof(H1SC)=Sof(H1SD)=1-FVAR(2)
 Sof(Cl1S)=Sof(Cl2S)=Sof(C1S)=Sof(H1SA)=Sof(H1SB)=FVAR(2)
 Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=1-FVAR(3)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C19(H19), C19'(H19'), C22(H22), C22'(H22')
6.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C5'(H5'A,H5'B), C9(H9A,H9B), C9'(H9'A,H9'B), C11(H11A,H11B),
 C11'(H11C,H11D), C1S(H1SA,H1SB), C1SB(H1SC,H1SD), C2S(H2SA,H2SB), C2S(H2SC,
 H2SD)
6.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C15'(H15'), C16(H16), C16'(H16'), C17(H17), C17'(H17')
6.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C7'(H7'A,H7'B,H7'C), C8(H8A,H8B,H8C), C8'(H8'A,H8'B,H8'C),
 C10(H10A,H10B,H10C), C10'(H10D,H10E,H10F), C12(H12A,H12B,H12C), C12'(H12D,H12E,
 H12F), C20(H20A,H20B,H20C), C20'(H20D,H20E,H20F), C21(H21A,H21B,H21C),
 C21'(H21D,H21E,H21F), C23(H23A,H23B,H23C), C23'(H23D,H23E,H23F), C24(H24A,H24B,
 H24C), C24'(H24D,H24E,H24F)
;
_shelx_res_checksum              98630
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'