Mono- and Digold(I) Complexes with Mesoionic Carbenes: Structural Characterization and Use in Catalytic Silver-Free Oxazoline Formation
Hettmanczyk, Lara; Schulze, Dennis; Suntrup, Lisa; Sarkar, Biprajit; Organometallics 35 (2016) 3828–; doi:10.1021/acs.organomet.6b00675

data_4089055
_publ_section_title
;
 Mono- and Digold(I) Complexes with Mesoionic Carbenes: Structural
 Characterization and Use in Catalytic Silver-Free Oxazoline Formation
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              3828
_journal_paper_doi               10.1021/acs.organomet.6b00675
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C21 H26 I N3'
_chemical_formula_weight         447.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8184(13)
_cell_length_b                   13.242(2)
_cell_length_c                   20.089(3)
_cell_measurement_reflns_used    4270
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.512
_cell_measurement_theta_min      1.842
_cell_volume                     2079.8(6)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart AXS'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13969
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.512
_diffrn_reflns_theta_min         1.842
_exptl_absorpt_coefficient_mu    1.547
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       block
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.376
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Flack x determined using 1669 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.002(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         4765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+1.7539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0794
_reflns_Friedel_coverage         0.752
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                4270
_reflns_number_total             4765
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00675_si_002.cif
_cod_data_source_block           sar324m
_cod_original_cell_volume        2079.9(6)
_cod_database_code               4089055
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              41139
_shelx_hkl_checksum              46122