Synthesis and Tunability of Abnormal 1,2,3-Triazolylidene Palladium and Rhodium Complexes
Poulain, Aurélie; Canseco-Gonzalez, Daniel; Hynes-Roche, Rachel; Müller-Bunz, Helge; Schuster, Oliver; Stoeckli-Evans, Helen; Neels, Antonia; Albrecht, Martin; Organometallics 30 (2011) 1021–; doi:10.1021/om101076u

data_4063994
_publ_section_title
;
 Synthesis and Tunability of Abnormal 1,2,3-Triazolylidene Palladium and
 Rhodium Complexes
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1021
_journal_paper_doi               10.1021/om101076u
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C22 H26 I4 N6 Pd2, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C22.5 H27 Cl I4 N6 Pd2'
_chemical_formula_weight         1137.35
_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                71.430(5)
_cell_angle_beta                 66.276(5)
_cell_angle_gamma                70.827(6)
_cell_formula_units_Z            2
_cell_length_a                   11.6395(8)
_cell_length_b                   13.1766(10)
_cell_length_c                   13.3346(9)
_cell_measurement_reflns_used    23718
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.53
_cell_measurement_theta_min      1.67
_cell_volume                     1726.9(2)
_computing_cell_refinement       'X-Area V1.35'
_computing_data_collection       'X-Area V1.35 (Stoe & Cie, 2006)'
_computing_data_reduction        'X-RED32 V1.31 (Stoe & Cie, 2006)'
_computing_molecular_graphics
'ORTEP3 (Farrugia, 1997), MERCURY (Macrea 2006), PLATON (Spek, 2009)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'phi + omega 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  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16880
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.715
_exptl_absorpt_correction_T_max  0.4747
_exptl_absorpt_correction_T_min  0.2380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULscanABS in PLATON (Spek, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.187
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1050
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
N: Total Potential Solvent Accessible Void Vol .   338.6 Ang^3
N: Electron Count / Cell =    115 
Equated to one half molecule of Dichloromethane per molecule of 
complex.
;
_refine_diff_density_max         0.844
_refine_diff_density_min         -1.003
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       0.00136(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         6105
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0517P)^2^+0.9776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0849
_reflns_number_gt                5157
_reflns_number_total             6105
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om101076u_si_002.cif
_cod_data_source_block           complex-2a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_formula_sum        'C22.50 H27 Cl I4 N6 Pd2'
_cod_database_code               4063994