η2-Allenyl- and η2-Alkynylphosphonium Complexes of Platinum
Colebatch, Annie L.; Cade, Ian A.; Hill, Anthony F.; Bhadbhade, Mohan M.; Organometallics 32 (2013) 4766–; doi:10.1021/om400406s

data_4081258
_publ_section_title
;
 \h2-Allenyl- and \h2-Alkynylphosphonium Complexes of Platinum
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4766
_journal_paper_doi               10.1021/om400406s
_journal_volume                  32
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_moiety         'C42 H38 F12 O1 P4'
_chemical_formula_sum            'C42 H38 F12 O P4'
_chemical_formula_weight         910.63
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2b'
_symmetry_space_group_name_H-M   'P b c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8056(2)
_cell_length_b                   15.8370(2)
_cell_length_c                   24.4050(3)
_cell_measurement_reflns_used    53233
_cell_measurement_temperature    200
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.55
_cell_volume                     4176.39(11)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows v. 2.01'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            51573
_diffrn_reflns_theta_full        25.021
_diffrn_reflns_theta_max         25.021
_diffrn_reflns_theta_min         2.572
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.939
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.24
_refine_diff_density_min         -0.20
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9801
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         7313
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.0223348
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 1.46P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0881
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0881
_reflns_limit_h_max              12
_reflns_limit_h_min              0
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              -28
_reflns_number_gt                6449
_reflns_number_total             7336
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.82
_oxford_diffrn_Wilson_scale      11.01
_oxford_refine_ls_r_factor_ref   0.0436
_oxford_refine_ls_scale          0.3813(4)
_oxford_reflns_number_all        7313
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            om400406s_si_002.cif
_cod_data_source_block           Compound_5
_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 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P b c 21 '
_cod_original_formula_sum        'C42 H38 F12 O1 P4'
_cod_database_code               4081258