Circumambulatory Rearrangement with Characteristics of a 2:1 Covalent Molecular Bevel Gear
Rosa E. Bulo; Florian Allaart; Andreas W. Ehlers; Franciscus J. J. de Kanter; Marius Schakel; Martin Lutz; Anthony L. Spek; Koop Lammertsma; Journal of the American Chemical Society 128 (2006) 12169–12173; doi:10.1021/ja0627895

data_4110867
_publ_contact_author_address
; Bijvoet Center for Biomolecular Research
  Dep. Crystal and Structural Chemistry
  Utrecht University
  Padualaan 8
  3584 CH Utrecht
  The Netherlands
;
_publ_contact_author_email       m.lutz@chem.uu.nl
_publ_contact_author_fax         '[+31] 30 2533940'
_publ_contact_author_name        'Martin Lutz'
_publ_contact_author_phone       '[+31] 30 2533902'
_publ_section_title
;
 Circumambulatory Rearrangement with Characteristics of a 2:1 Covalent
 Molecular Bevel Gear
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12169
_journal_page_last               12173
_journal_paper_doi               10.1021/ja0627895
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C14 H11 O5 P W'
_chemical_formula_sum            'C14 H11 O5 P W'
_chemical_formula_weight         474.05
_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   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.442(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0373(11)
_cell_length_b                   13.4576(11)
_cell_length_c                   13.5480(11)
_cell_measurement_reflns_used    92
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.75
_cell_measurement_theta_min      3.84
_cell_volume                     1544.0(3)
_computing_cell_refinement       Dirax
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'EvalCCD, ABST, Sortav'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-97 (Beurskens et al., 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            20279
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    7.601
_exptl_absorpt_correction_T_max  0.37
_exptl_absorpt_correction_T_min  0.17
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.039
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.606
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         3522
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0177
_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^)+(0.0225P)^2^+1.0800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0432
_refine_ls_wR_factor_ref         0.0448
_reflns_number_gt                3192
_reflns_number_total             3522
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja0627895si20060501_050610_2.cif
_cod_data_source_block           s2938a
_cod_original_cell_volume        1543.9(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4110867