Platinum(II) and Palladium(II) Dibenzo[a,e]cyclooctatetraene (DBCOT) Oxo and Halide Complexes: Comparison to 1,5-COD Analogues
Singh, Anupam; Sharp, Paul R.; Organometallics 25 (2006) 678–; doi:10.1021/om050713w

data_4074655
_publ_section_title
;
 Platinum(II) and Palladium(II) Dibenzo[a,e]cyclooctatetraene (DBCOT) Oxo
 and Halide Complexes:&#x00A0; Comparison to 1,5-COD Analogues
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              678
_journal_paper_doi               10.1021/om050713w
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety
'C102 H81 Au3 O3 P3 Pt3 3+, 3(B1 F4 1-), 10(CH Cl3)'
_chemical_formula_sum            'C112 H91 Au3 B3 Cl30 F12 O3 P3 Pt3'
_chemical_formula_weight         4077.86
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 97.8320(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5038(9)
_cell_length_b                   36.472(2)
_cell_length_c                   26.1887(16)
_cell_measurement_reflns_used    9839
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.75
_cell_measurement_theta_min      2.23
_cell_volume                     13724.1(14)
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics
;
 L. J. Barbour, X-Seed - Graphical Interface to
 SHELX-97 and POV-Ray, 1999
;
_computing_publication_material  WinGX
_computing_structure_refinement
;
 SHELXL-97 (Sheldrick, 1997), L. J. Barbour, X-Seed - Graphical Interface to
 SHELX-97 and POV-Ray, 1999
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1784
_diffrn_reflns_av_sigmaI/netI    0.2107
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            81367
_diffrn_reflns_theta_full        24.76
_diffrn_reflns_theta_max         24.76
_diffrn_reflns_theta_min         1.42
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    6.924
_exptl_absorpt_correction_T_max  0.4232
_exptl_absorpt_correction_T_min  0.2764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Data were corrected for decay and absorption using the program SADABS 
 based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995).   
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.974
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             7744
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.923
_refine_diff_density_min         -2.957
_refine_diff_density_rms         0.340
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1353
_refine_ls_number_reflns         23431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1862
_refine_ls_R_factor_gt           0.0827
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0939P)^2^+82.1674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1808
_refine_ls_wR_factor_ref         0.2246
_reflns_number_gt                12158
_reflns_number_total             23431
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050713wsi20050817_125723.cif
_cod_data_source_block           '[(DBCOT)Pt(O)AuPPh3]3(BF4)3_(6)'
_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 
;
_cod_original_cell_volume        13724.0(15)
_cod_original_sg_symbol_H-M      'P2(1)/c  '
_cod_database_code               4074655