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_4086968
_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_sum            'C21 H25 Br2 Cl2 N3 O Pd'
_chemical_formula_weight         672.56
_chemical_name_systematic
; 
 ? 
;
_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   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                81.042(5)
_cell_angle_beta                 78.122(4)
_cell_angle_gamma                81.507(5)
_cell_formula_units_Z            2
_cell_length_a                   9.0934(13)
_cell_length_b                   9.9794(15)
_cell_length_c                   14.098(2)
_cell_measurement_reflns_used    9497
_cell_measurement_temperature    99(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.31
_cell_volume                     1227.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      99(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            52208
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.305
_exptl_absorpt_coefficient_mu    4.246
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6230
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.819
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Plate
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.803
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         5635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0223
_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^)+(0.0341P)^2^+0.9260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0561
_refine_ls_wR_factor_ref         0.0580
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5100
_reflns_number_total             5635
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00736_si_002.cif
_cod_data_source_block           cis-1
_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.

'_exptl_crystal_density_meas' value 'Not Measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_database_code               4086968
_shelxl_version_number           2013-3
_shelx_res_checksum              95237
_shelx_hkl_checksum              87648