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_1540543
_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, 3.5(C4 H8 O)'
_chemical_formula_sum            'C60 H98 Au N2 O3.5'
_chemical_formula_weight         1100.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 119.0230(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0066(6)
_cell_length_b                   16.2975(5)
_cell_length_c                   20.6068(6)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.119
_cell_measurement_theta_min      2.260
_cell_volume                     5875.3(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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II TXS'
_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  0.0557
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35165
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.374
_diffrn_reflns_theta_max         25.374
_diffrn_reflns_theta_min         2.261
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.547
_exptl_absorpt_correction_T_max  0.4901
_exptl_absorpt_correction_T_min  0.4123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.0973 before and 0.0611 after correction.
The Ratio of minimum to maximum transmission is 0.8413.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_description       Block
_exptl_crystal_F_000             2316
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.103
_refine_diff_density_max         0.591
_refine_diff_density_min         -1.048
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         5391
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0422P)^2^+29.1045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1209
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4675
_reflns_number_total             5391
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03654b2.cif
_cod_data_source_block           MM57
_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_original_formula_sum        'C60 H98 Au N2 O3.50'
_cod_database_code               1540543
_shelx_estimated_absorpt_t_max   0.779
_shelx_estimated_absorpt_t_min   0.625
_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. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(Au1) = Uanis(C2)
3. Others
 Fixed Sof: Au1(0.5) C2(0.5) C1(0.5)
4.a Ternary CH refined with riding coordinates:
 C19(H19), C22(H22)
4.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C9(H9A,H9B), C11(H11A,H11B)
4.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C17(H17)
4.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C20(H20A,H20B,
 H20C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,
 H12C)
;
_shelx_res_checksum              16944
_shelx_fab_checksum              25431
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'