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_4078849
_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         'C38 H43 I2 N5 P Pd, 2(C2 H3 N), I'
_chemical_formula_sum            'C42 H49 I3 N7 P Pd'
_chemical_formula_weight         1169.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.906(3)
_cell_angle_beta                 88.010(3)
_cell_angle_gamma                86.666(3)
_cell_formula_units_Z            4
_cell_length_a                   13.782(3)
_cell_length_b                   15.694(3)
_cell_length_c                   22.394(5)
_cell_measurement_reflns_used    6916
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.90
_cell_measurement_theta_min      2.25
_cell_volume                     4759.2(17)
_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 0.985
_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  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            42692
_diffrn_reflns_theta_full        27.64
_diffrn_reflns_theta_max         27.64
_diffrn_reflns_theta_min         0.92
_exptl_absorpt_coefficient_mu    2.405
_exptl_absorpt_correction_T_max  0.8771
_exptl_absorpt_correction_T_min  0.3934
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.06
_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 
University, Utrecht, The Netherlands).  A total solvent-accessible 
void volume of 199 cubic Angstroms with a total electron count of 45
(consistent with 2 molecule of solvent acetonitrile, or 0.5 molecule per
formula unit of the palladium complex) was found in the unit cell.
;
_refine_diff_density_max         1.063
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     951
_refine_ls_number_reflns         21838
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+2.5075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0924
_reflns_number_gt                16825
_reflns_number_total             21838
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om3004543_si_003.cif
_cod_data_source_block           10b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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        4759.3(17)
_cod_database_code               4078849