Synthesis and Structure of Silver and Rhodium 1,2,3-Triazol-5-ylidene Mesoionic Carbene Complexes
Keske, Eric C.; Zenkina, Olena V.; Wang, Ruiyao; Crudden, Cathleen M.; Organometallics 31 (2012) 456–; doi:10.1021/om201104f

data_4068121
_publ_section_title
;
 Synthesis and Structure of Silver and Rhodium 1,2,3-Triazol-5-ylidene
 Mesoionic Carbene Complexes
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              456
_journal_paper_doi               10.1021/om201104f
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C57 H76 B2 Cl2 F8 N8 Rh2'
_chemical_formula_weight         1323.60
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 128.050(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.7866(9)
_cell_length_b                   34.3081(17)
_cell_length_c                   13.4527(7)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.14
_cell_measurement_theta_min      2.26
_cell_volume                     6464.5(6)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0238
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29669
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.657
_exptl_absorpt_correction_T_max  0.9806
_exptl_absorpt_correction_T_min  0.8272
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.102
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         6331
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0675P)^2^+20.7660P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1276
_reflns_number_gt                5350
_reflns_number_total             6331
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201104f_si_002.cif
_cod_data_source_block           cc98
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4068121