Oxidative Dehydrogenation of Tris(o-isopropylphenyl)phosphines by Platinum Complexes
Baber, Angharad; Fan, Cheng; Norman, David W.; Orpen, A. Guy; Pringle, Paul G.; Wingad, Richard L.; Organometallics 27 (2008) 5906–; doi:10.1021/om800382m

data_4071781
_publ_section_title
;
 Oxidative Dehydrogenation of Tris(o-isopropylphenyl)phosphines by
 Platinum Complexes
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5906
_journal_paper_doi               10.1021/om800382m
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C30 H35 Cl4 O3 P Pt'
_chemical_formula_sum            'C30 H35 Cl4 O3 P Pt'
_chemical_formula_weight         811.47
_chemical_name_systematic
; 
 ? 
;
_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                 109.57(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.348(3)
_cell_length_b                   15.743(3)
_cell_length_c                   15.330(3)
_cell_measurement_reflns_used    6966
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.04
_cell_measurement_theta_min      2.59
_cell_volume                     3035.3(12)
_computing_cell_refinement       'SMART v5.628 (Bruker-AXS, 1997-2002)'
_computing_data_collection       'SMART v5.628 (Bruker-AXS, 1997-2002)'
_computing_data_reduction
; 
 SAINT v7.06A (Bruker-AXS, 1997-2003) & SHELXTL v6.14 (Bruker-AXS, 2003) 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.366
_diffrn_detector_type            'Bruker-AXS SMART APEX'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      'frames, 0.3\% width'
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker-AXS D8'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'glass fibre'
_diffrn_radiation_collimation    monocap
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71074
_diffrn_reflns_av_R_equivalents  0.1058
_diffrn_reflns_av_sigmaI/netI    0.0814
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34003
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.62
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           40
_diffrn_source_power             2
_diffrn_source_target            Mo
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    5.059
_exptl_absorpt_correction_T_max  0.414
_exptl_absorpt_correction_T_min  0.362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10 (Sheldrick, G.M., 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         4.729
_refine_diff_density_min         -4.792
_refine_diff_density_rms         0.281
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.274
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         6966
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.274
_refine_ls_R_factor_all          0.1131
_refine_ls_R_factor_gt           0.0951
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+63.6320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1837
_refine_ls_wR_factor_ref         0.1924
_reflns_number_gt                5874
_reflns_number_total             6966
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800382m_si_003.cif
_cod_data_source_block           2c_ptmethom
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' 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        3035.4(11)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4071781