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_4067411
_publ_section_title
;
 Partial Ring-Opening and Rearrangement Reactions of P,C-Cages to Yield
 Unusual Phosphinous Acids Stabilized by Pentacarbonyltungsten
;
_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         'C21 H23 O10 P W, C D Cl3'
_chemical_formula_sum            'C22 H23 Cl3 D O10 P W'
_chemical_formula_weight         770.59
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 98.664(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0292(4)
_cell_length_b                   18.2659(6)
_cell_length_c                   12.7250(3)
_cell_measurement_reflns_used    15826
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     2764.08(15)
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_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  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18933
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    4.578
_exptl_absorpt_correction_T_max  0.3651
_exptl_absorpt_correction_T_min  0.1646
_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    1.852
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pillar
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.617
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.171
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         5992
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0194
_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^)+(0.0085P)^2^+1.5840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0419
_refine_ls_wR_factor_ref         0.0429
_reflns_number_gt                5323
_reflns_number_total             5992
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9009334_si_002.cif
_cod_data_source_block           joerg23
_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 
;
_cod_original_cell_volume        2764.08(14)
_cod_original_sg_symbol_H-M      P21/n
_cod_original_formula_sum        'C22 H23 D Cl3 O10 P W'
_cod_database_code               4067411