A simple access to transition metal cyclopropenylidene complexes
Yannick D. Bidal; Mathieu Lesieur; Mohand Melaimi; David B. Cordes; Alexandra M. Z. Slawin; Guy Bertrand; Catherine S. J. Cazin; Chem.Commun. 51 (2015) 4778–; doi:10.1039/C4cc10375K

data_7116712
_publ_section_title
;
 A simple access to transition metal cyclopropenylidene complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              4778
_journal_paper_doi               10.1039/C4cc10375K
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C30 H56 Au N4, 0.5(O6 S2), 0.5(C2 F6)'
_chemical_formula_sum            'C31 H56 Au F3 N4 O3 S'
_chemical_formula_weight         818.82
_chemical_melting_point          485
_chemical_name_systematic        '[Au(BAC)2][OTf] '
_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             2014-07-28
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2014-08-22 deposited with the CCDC.
2015-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.610(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.2941(6)
_cell_length_b                   9.5096(5)
_cell_length_c                   14.5324(7)
_cell_measurement_reflns_used    7918
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.416
_cell_measurement_theta_min      2.561
_cell_volume                     1833.56(15)
_computing_cell_refinement       'SAINT v8.18C (Bruker, 2012)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.18C (Bruker, 2012)'
_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 Photon-100 area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'four-circle KAPPA diffractometer'
_diffrn_measurement_device_type  'Bruker Photon100 Imus'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12626
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.417
_diffrn_reflns_theta_min         2.561
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mus'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.118
_exptl_absorpt_correction_T_max  0.0932
_exptl_absorpt_correction_T_min  0.0363
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1629 before and 0.0805 after correction. The Ratio of minimum to maximum transmission is 0.3895. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            Colorless
_exptl_crystal_colour_primary    Colorless
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       Plate
_exptl_crystal_F_000             832
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethyl ether/dichloromethane'
_exptl_crystal_size_max          0.105
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.032
_refine_diff_density_max         0.895
_refine_diff_density_min         -1.243
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         3719
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.201
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0377
_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^)+10.2416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.0993
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3215
_reflns_number_total             3719
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc10375k2.cif
_cod_data_source_block           MM2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 
;
_cod_database_code               7116712
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.880
_shelx_estimated_absorpt_t_min   0.672
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{S1A, C1A}
{O1A, F1A}
{O2A, F2A}
{O3A, F3A}
3. Uiso/Uaniso restraints and constraints
Uanis(S1A) = Uanis(C1A)
Uanis(O1A) = Uanis(F1A)
Uanis(O2A) = Uanis(F2A)
Uanis(O3A) = Uanis(F3A)
4. Others
 Fixed Sof: S1A(0.5) O1A(0.5) O2A(0.5) O3A(0.5) C1A(0.5) F1A(0.5) F2A(0.5)
 F3A(0.5)
5.a Ternary CH refined with riding coordinates:
 C6(H6), C8(H8), C10(H10), C13(H13)
5.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C11(H11A,
 H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              99291
_olex2_submission_special_instructions 'No special instructions were received'