Complexation of (5H)-Dibenzo[a,d]cyclohepten-5-ylidene to Palladium(II) via the Diazo Route and Evidence of C−H···Pd Interactions
Taubmann, Christian; Öfele, Karl; Herdtweck, Eberhardt; Herrmann, Wolfgang A.; Organometallics 28 (2009) 4254–; doi:10.1021/om900266z

data_4069549
_publ_section_title
;
 Complexation of (5H)-Dibenzo[a,d]cyclohepten-5-ylidene to Palladium(II)
 via the Diazo Route and Evidence of C&#x2212;H&#x00B7;&#x00B7;&#x00B7;Pd
 Interactions
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4254
_journal_paper_doi               10.1021/om900266z
_journal_volume                  28
_journal_year                    2009
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C33 H25 Cl2 P Pd, C H2 Cl2'
_chemical_formula_sum            'C34 H27 Cl4 P Pd'
_chemical_formula_weight         714.75
_chemical_name_systematic        ?
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      29
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.2199(4)
_cell_length_b                   17.5722(4)
_cell_length_c                   16.9145(4)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      67.21
_cell_measurement_theta_min      2.51
_cell_volume                     6009.9(2)
_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, 2008)'
_computing_publication_material  'PLATON (Spek, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1998)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      173(1)
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.764
_diffrn_measured_fraction_theta_max 0.764
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker \k-CCD diffractometer'
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
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_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            58303
_diffrn_reflns_theta_full        67.21
_diffrn_reflns_theta_max         67.21
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    8.934
_exptl_absorpt_correction_T_max  0.4894
_exptl_absorpt_correction_T_min  0.3061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, G. (Bruker, 2008b)'
_exptl_crystal_colour            red
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_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
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_refine_ls_extinction_method     none
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_refine_ls_number_reflns         8220
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_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+8.0943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                7357
_reflns_number_total             8220
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om900266z_si_002.cif
_cod_data_source_block           TAUN-7009-173
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 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_database_code               4069549