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_4063995
_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         'C14 H26 I4 N6 Pd2'
_chemical_formula_sum            'C14 H26 I4 N6 Pd2'
_chemical_formula_weight         998.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 92.469(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.6739(15)
_cell_length_b                   14.442(2)
_cell_length_c                   11.515(3)
_cell_measurement_reflns_used    3519
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.34
_cell_measurement_theta_min      2.26
_cell_volume                     1275.0(5)
_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    'PLATON  (Spek, 2009)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.2046
_diffrn_reflns_av_sigmaI/netI    0.1569
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9417
_diffrn_reflns_theta_full        25.21
_diffrn_reflns_theta_max         25.21
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.264
_exptl_absorpt_correction_T_max  0.410
_exptl_absorpt_correction_T_min  0.028
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'DELrefABS in PLATON; Spek, 2009'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.602
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.068
_refine_diff_density_min         -1.472
_refine_diff_density_rms         0.292
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.837
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         2254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.837
_refine_ls_R_factor_all          0.1487
_refine_ls_R_factor_gt           0.0836
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1249P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2110
_refine_ls_wR_factor_ref         0.2486
_reflns_number_gt                903
_reflns_number_total             2254
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om101076u_si_002.cif
_cod_data_source_block           complex-2b
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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_sg_symbol_H-M      'P 21/n'
_cod_database_code               4063995