[2+2] Cycloaddition Reactions with a Tungsten-Stabilized 2H-Phenol
Michael A. Todd; Michal Sabat; William H. Myers; W. Dean Harman; Journal of the American Chemical Society 129 (2007) 11010–11011; doi:10.1021/ja0739279

data_4109917
_publ_section_title
;
 [2+2] Cycloaddition Reactions with a Tungsten-Stabilized 2H-Phenol
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11010
_journal_page_last               11011
_journal_paper_doi               10.1021/ja0739279
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C29.5 H37.5 B Cl7.5 N7 O4 P W'
_chemical_formula_weight         1045.67
_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                69.54(2)
_cell_angle_beta                 68.67(2)
_cell_angle_gamma                69.36(2)
_cell_formula_units_Z            4
_cell_length_a                   16.871(3)
_cell_length_b                   17.435(3)
_cell_length_c                   17.808(3)
_cell_measurement_reflns_used    8164
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      31.603
_cell_measurement_theta_min      3.645
_cell_volume                     4416.5(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART APEX 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  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0739
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            75292
_diffrn_reflns_theta_full        36.41
_diffrn_reflns_theta_max         36.41
_diffrn_reflns_theta_min         2.82
_exptl_absorpt_coefficient_mu    3.146
_exptl_absorpt_correction_T_max  0.810981
_exptl_absorpt_correction_T_min  0.524566
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       block
_exptl_crystal_F_000             2068
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.029
_refine_diff_density_min         0.679
_refine_diff_density_rms         0.137
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     953
_refine_ls_number_reflns         42775
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.0726
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1082P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2031
_refine_ls_wR_factor_ref         0.2272
_reflns_number_gt                26764
_reflns_number_total             42775
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0739279si20070614_074718.cif
_cod_data_source_block           C27H35BN7O4PW_2.5CHCl3
_cod_original_cell_volume        4416.4(14)
_cod_original_formula_sum        'C29.50 H37.50 B Cl7.50 N7 O4 P W'
_cod_database_code               4109917