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_4067408
_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         'C26 H25 O7 P W'
_chemical_formula_sum            'C26 H25 O7 P W'
_chemical_formula_weight         664.28
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 120.6280(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.9185(12)
_cell_length_b                   8.9633(2)
_cell_length_c                   20.9422(8)
_cell_measurement_reflns_used    16461
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     5317.1(3)
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0545
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            22141
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    4.446
_exptl_absorpt_correction_T_max  0.42467
_exptl_absorpt_correction_T_min  0.24781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            'light yellowish'
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rhombic plate'
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.681
_refine_diff_density_min         -2.143
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         6972
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0253P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0657
_reflns_number_gt                5143
_reflns_number_total             6972
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9009334_si_002.cif
_cod_data_source_block           greg266
_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.

'_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 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4067408