Partial Ring-Opening and Rearrangement Reactions of P,C-Cages to Yield Unusual Phosphinous Acids Stabilized by Pentacarbonyltungsten
Bode, Maren; Schnakenburg, Gregor; Daniels, Jörg; Marinetti, Angela; Streubel, Rainer; Organometallics 29 (2010) 656–; doi:10.1021/om9009334

data_4067407
_publ_section_title
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 Partial Ring-Opening and Rearrangement Reactions of P,C-Cages to Yield
 Unusual Phosphinous Acids Stabilized by Pentacarbonyltungsten
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_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              656
_journal_paper_doi               10.1021/om9009334
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C20 H21 O7 P W'
_chemical_formula_sum            'C20 H21 O7 P W'
_chemical_formula_weight         588.19
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                75.655(2)
_cell_angle_beta                 83.494(2)
_cell_angle_gamma                70.934(2)
_cell_formula_units_Z            4
_cell_length_a                   10.7147(5)
_cell_length_b                   13.2996(5)
_cell_length_c                   16.8471(5)
_cell_measurement_reflns_used    8042
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      1.00
_cell_volume                     2196.92(15)
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1322
_diffrn_reflns_av_sigmaI/netI    0.1158
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27583
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    5.368
_exptl_absorpt_correction_T_max  0.55720
_exptl_absorpt_correction_T_min  0.28406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.707
_refine_diff_density_min         -3.634
_refine_diff_density_rms         0.232
_refine_ls_extinction_coef       0.00086(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         10518
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1282
_reflns_number_gt                7083
_reflns_number_total             10518
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9009334_si_002.cif
_cod_data_source_block           greg1004
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' 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 
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_cod_database_code               4067407