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_7052706
_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           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.883(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.3643(8)
_cell_length_b                   6.6200(3)
_cell_length_c                   20.5323(8)
_cell_measurement_reflns_used    9380
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      39.27
_cell_measurement_theta_min      2.12
_cell_volume                     2741.8(2)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0772
_diffrn_reflns_av_sigmaI/netI    0.0804
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            45737
_diffrn_reflns_theta_full        35.00
_diffrn_reflns_theta_max         35.00
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    8.628
_exptl_absorpt_correction_T_max  0.2772
_exptl_absorpt_correction_T_min  0.1689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_refine_diff_density_max         4.363
_refine_diff_density_min         -3.833
_refine_diff_density_rms         0.310
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         12043
_refine_ls_number_restraints     287
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+3.6361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1188
_reflns_number_gt                9836
_reflns_number_total             12043
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1nj20087a.txt
_cod_data_source_block           mat51r
_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.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7052706