Intramolecular [4+2] versus [2+2] cycloadditions in P‒X‒P-linked biphospholes (X = O, S)
Duffy, Matthew P.; Lin, Yuhan; Ting, Liow Yu; Mathey, François; New Journal of Chemistry 35 (2011) 2001–; doi:10.1039/c1nj20087a

data_7052707
_publ_section_title
;
 Intramolecular [4+2] versus [2+2] cycloadditions in P--X--P-linked
 biphospholes (X = O, S)
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2001
_journal_paper_doi               10.1039/c1nj20087a
_journal_volume                  35
_journal_year                    2011
_chemical_formula_moiety         'C22 H16 O10 P2 S W2'
_chemical_formula_sum            'C22 H16 O10 P2 S W2'
_chemical_formula_weight         902.05
_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                97.99
_cell_angle_beta                 98.7280(10)
_cell_angle_gamma                98.47
_cell_formula_units_Z            2
_cell_length_a                   8.34540(10)
_cell_length_b                   9.55690(10)
_cell_length_c                   17.2960(2)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      31.05
_cell_measurement_theta_min      2.51
_cell_volume                     1330.12(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22739
_diffrn_reflns_theta_full        31.08
_diffrn_reflns_theta_max         31.08
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    8.892
_exptl_absorpt_correction_T_max  0.4150
_exptl_absorpt_correction_T_min  0.1251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.209
_refine_diff_density_min         -1.433
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         8467
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0209
_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^)+(0.0132P)^2^+1.2235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0472
_refine_ls_wR_factor_ref         0.0488
_reflns_number_gt                7569
_reflns_number_total             8467
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1nj20087a.txt
_cod_data_source_block           mat54s
_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 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7052707