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_4078848
_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 H28 I3 N5 Pd, 4(C2 H3 N)'
_chemical_formula_sum            'C28 H40 I3 N9 Pd'
_chemical_formula_weight         989.79
_chemical_name_systematic
; 
 ? 
;
_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                 119.530(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.695(19)
_cell_length_b                   17.496(11)
_cell_length_c                   15.149(9)
_cell_measurement_reflns_used    2599
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      18.95
_cell_measurement_theta_min      2.34
_cell_volume                     7079(8)
_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    'SIR-97 (Altomare et al, 1999)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0871
_diffrn_reflns_av_sigmaI/netI    0.0772
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26866
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    3.173
_exptl_absorpt_correction_T_max  0.7568
_exptl_absorpt_correction_T_min  0.2515
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             3808
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
Attempts to refine peaks of residual electron density as disordered or 
partial-occupancy solvent acetonitrile nitrogen or carbon atoms were 
unsuccessful.  The data were corrected for disordered electron density 
through use of the SQUEEZE procedure (Sluis, P. van der; Spek, A. L. 
Acta Crystallogr. 1990, A46, 194-201) as implemented in PLATON (Spek, 
A. L. Acta Crystallogr. 1990, A46, C34; Spek, A. L. J. Appl. Cryst. 2003, 
36, 7-13.  PLATON - a multipurpose crystallographic tool.  Utrecht 
niversity, Utrecht, The Netherlands).  A total solvent-accessible void 
volume of 1470 cubic Angstroms with a total electron count of 519
(consistent with 24 molecules of solvent acetonitrile, or 3 molecules
per formula unit of the palladium complex) was found in the unit cell.
;
_refine_diff_density_max         2.100
_refine_diff_density_min         -1.451
_refine_diff_density_rms         0.263
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         7143
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0734
_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^)+(0.1220P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1986
_refine_ls_wR_factor_ref         0.2186
_reflns_number_gt                4484
_reflns_number_total             7143
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om3004543_si_003.cif
_cod_data_source_block           7b
_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_cell_volume        7079(7)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4078848