Unsymmetrical Dicarbenes Based onN-Heterocyclic/Mesoionic Carbene Frameworks: A Stepwise Metalation Strategy for the Generation of a Dicarbene-Bridged Mixed-Metal Pd/Rh Complex
Zamora, Matthew T.; Ferguson, Michael J.; McDonald, Robert; Cowie, Martin; Organometallics 31 (2012) 5463–; doi:10.1021/om3004543

data_4078846
_publ_section_title
;
 Unsymmetrical Dicarbenes Based onN-Heterocyclic/Mesoionic Carbene
 Frameworks: A Stepwise Metalation Strategy for the Generation of a
 Dicarbene-Bridged Mixed-Metal Pd/Rh Complex
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              5463
_journal_paper_doi               10.1021/om3004543
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C20 H29 N5, 2(C F3 O3 S)'
_chemical_formula_sum            'C22 H29 F6 N5 O6 S2'
_chemical_formula_weight         637.62
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.3006(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.5497(7)
_cell_length_b                   14.4945(7)
_cell_length_c                   12.9298(6)
_cell_measurement_reflns_used    7376
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.61
_cell_measurement_theta_min      2.33
_cell_volume                     2847.3(2)
_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      173(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       '\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  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0219
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22483
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_T_max  0.9892
_exptl_absorpt_correction_T_min  0.8832
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         5831
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+1.7352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0968
_reflns_number_gt                4762
_reflns_number_total             5831
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om3004543_si_003.cif
_cod_data_source_block           4b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4078846