Donor Strength Determination of Benzoxazolin-2-ylidene, Benzobisoxazolin-2-ylidene, and Their Isocyanide Precursors by 13C NMR Spectroscopy of Their PdII and AuI Complexes
Meier, Martin; Tan, Tristan Tsai Yuan; Hahn, F. Ekkehardt; Huynh, Han Vinh; Organometallics 36 (2017) 275–; doi:10.1021/acs.organomet.6b00736

data_4086971
_publ_section_title
;
 Donor Strength Determination of Benzoxazolin-2-ylidene,
 Benzobisoxazolin-2-ylidene, and Their Isocyanide Precursors by 13C NMR
 Spectroscopy of Their PdII and AuI Complexes
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              275
_journal_paper_doi               10.1021/acs.organomet.6b00736
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C34 H40 Au2 N6 O2, 2(C4 H8 O), C2 H6 O'
_chemical_formula_sum            'C44 H62 Au2 F12 N6 O5 P2'
_chemical_formula_weight         1438.87
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                69.6340(10)
_cell_angle_beta                 88.1030(10)
_cell_angle_gamma                77.3010(10)
_cell_formula_units_Z            1
_cell_length_a                   10.5600(2)
_cell_length_b                   10.6675(2)
_cell_length_c                   12.8860(3)
_cell_measurement_reflns_used    12513
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.54
_cell_volume                     1326.07(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  'Goebel mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17831
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         3.111
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    5.676
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Multi-scan correction included in APEX2 package (Bruker AXS, 2012)
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_description       Block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.401
_exptl_crystal_size_mid          0.265
_exptl_crystal_size_min          0.155
_refine_diff_density_max         3.624
_refine_diff_density_min         -1.007
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5404
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0430P)^2^+4.2262P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.0934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5138
_reflns_number_total             5404
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00736_si_002.cif
_cod_data_source_block           '[9](PF6)2'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/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 
;
_cod_database_code               4086971
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.209
_shelx_estimated_absorpt_t_max   0.473
_shelx_res_checksum              55401
_shelx_hkl_checksum              1805