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_4064001
_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_sum            'C23 H28 Cl2 I2 N6 Pd'
_chemical_formula_weight         819.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 112.592(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7461(9)
_cell_length_b                   17.2912(9)
_cell_length_c                   14.1530(10)
_cell_measurement_reflns_used    22444
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.58
_cell_measurement_theta_min      1.73
_cell_volume                     2879.9(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_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  0.0892
_diffrn_reflns_av_sigmaI/netI    0.0590
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28970
_diffrn_reflns_theta_full        25.17
_diffrn_reflns_theta_max         25.17
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    2.997
_exptl_absorpt_correction_T_max  0.520
_exptl_absorpt_correction_T_min  0.369
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULscanABS, (PLATON03, Speck, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.890
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.880
_refine_diff_density_min         -1.087
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         5134
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0628P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.0989
_reflns_number_gt                3814
_reflns_number_total             5134
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101076u_si_002.cif
_cod_data_source_block           complex_cis3a_pentane
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4064001