Reactions of Nitrogen Donors with Cycloheptatrienylidene Complexes: Metal Coordination versus Nucleophilic Attack on the Carbene Ligand
Mantas-Öktem, Kevser; Öfele, Karl; Pöthig, Alexander; Bechlars, Bettina; Herrmann, Wolfgang A.; Kühn, Fritz E.; Organometallics 31 (2012) 8249–; doi:10.1021/om300867g

data_4079588
_publ_section_title
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 Reactions of Nitrogen Donors with Cycloheptatrienylidene Complexes: Metal
 Coordination versus Nucleophilic Attack on the Carbene Ligand
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              8249
_journal_paper_doi               10.1021/om300867g
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C11 H12 Br2 N2 Pd'
_chemical_formula_sum            'C11 H12 Br2 N2 Pd'
_chemical_formula_weight         438.43
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                87.7186(13)
_cell_angle_beta                 88.2397(12)
_cell_angle_gamma                80.5587(13)
_cell_formula_units_Z            2
_cell_length_a                   5.6405(2)
_cell_length_b                   8.1669(3)
_cell_length_c                   14.2380(5)
_cell_measurement_reflns_used    9809
_cell_measurement_temperature    123
_cell_measurement_theta_max      31.4716
_cell_measurement_theta_min      2.5297
_cell_volume                     646.29(4)
_computing_cell_refinement       'SAINT (Bruker, 2008b)'
_computing_data_collection       'APEX II Control Software (Bruker, 2008a)'
_computing_data_reduction        'SAINT (Bruker, 2008b)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed-tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0148
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14415
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    7.592
_exptl_absorpt_correction_T_max  0.394
_exptl_absorpt_correction_T_min  0.189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_crystal_colour            'clear intense orange-brown '
_exptl_crystal_density_diffrn    2.253
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2350
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0142
_refine_ls_R_factor_gt           0.0127
_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^)+(0.0098P)^2^+0.3937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0286
_refine_ls_wR_factor_ref         0.0291
_reflns_number_gt                2243
_reflns_number_total             2350
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om300867g_si_002.cif
_cod_data_source_block           7
_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 
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_cod_database_code               4079588