Synthesis of Novel O,P,C-Cage Complexes via Thermal C−O Ring Opening of an Oxaphosphirane W(CO)5Complex
Bode, Maren; Schnakenburg, Gregor; Jones, Peter G.; Streubel, Rainer; Organometallics 27 (2008) 2664–; doi:10.1021/om7012953

data_4071151
_publ_section_title
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 Synthesis of Novel O,P,C-Cage Complexes via Thermal C&#x2212;O Ring
 Opening of an Oxaphosphirane W(CO)5Complex
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_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2664
_journal_paper_doi               10.1021/om7012953
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C29 H27 O7 P W'
_chemical_formula_weight         702.33
_chemical_name_systematic
;
 ?
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.218(4)
_cell_angle_beta                 105.029(4)
_cell_angle_gamma                93.583(4)
_cell_formula_units_Z            2
_cell_length_a                   8.8233(8)
_cell_length_b                   10.7260(10)
_cell_length_c                   15.0798(14)
_cell_measurement_reflns_used    7775
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      30.55
_cell_measurement_theta_min      2.30
_cell_volume                     1373.4(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29773
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.57
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    4.309
_exptl_absorpt_correction_T_max  0.5642
_exptl_absorpt_correction_T_min  0.4608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.142
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         8358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0169
_refine_ls_R_factor_gt           0.0152
_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^)+(0.0202P)^2^+0.3659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0369
_refine_ls_wR_factor_ref         0.0375
_reflns_number_gt                7925
_reflns_number_total             8358
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7012953-file004.cif
_cod_data_source_block           tuete
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4071151