Remarkable Metal-Complexed Phosphorus Analogues of the Cyclopropenylcarbene-Cyclobutadiene Rearrangement
Volodymyr Lyaskovskyy; Niels Elders; Andreas W. Ehlers; Martin Lutz; J. Chris Slootweg; Koop Lammertsma; Journal of the American Chemical Society 133 (2011) 9704–9707; doi:10.1021/ja203083c

data_4106323
_publ_contact_author_address
; Bijvoet Center for Biomolecular Research
  Crystal and Structural Chemistry
  Utrecht University
  Padualaan 8
  3584 CH Utrecht
  The Netherlands
;
_publ_contact_author_email       m.lutz@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
;
 Remarkable Metal-Complexed Phosphorus Analogues of the
 Cyclopropenylcarbene-Cyclobutadiene Rearrangement
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9704
_journal_page_last               9707
_journal_paper_doi               10.1021/ja203083c
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C19 H27 O4 P W'
_chemical_formula_sum            'C19 H27 O4 P W'
_chemical_formula_weight         534.23
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.47483(15)
_cell_length_b                   16.83580(7)
_cell_length_c                   9.7775(3)
_cell_measurement_reflns_used    24130
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.08
_cell_volume                     2053.51(7)
_computing_cell_refinement       Peakref
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Eval14, Sadabs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0084
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            41367
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    5.722
_exptl_absorpt_correction_T_max  0.5477
_exptl_absorpt_correction_T_min  0.1190
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_description       plate
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.845
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       0.00099(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2437
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.0144
_refine_ls_R_factor_gt           0.0113
_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^)+(0.0071P)^2^+1.3534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0237
_refine_ls_wR_factor_ref         0.0246
_reflns_number_gt                2212
_reflns_number_total             2437
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja203083c_si_002_1.cif
_cod_data_source_block           s4298a
_cod_database_code               4106323