Annelation of Phosphole-Substituted Fischer Carbene Complexes by Alkynes
Ng, Kim Hong; Li, Yongxin; Ganguly, Rakesh; Mathey, Francois; Organometallics 32 (2013) 7482–; doi:10.1021/om4009795

data_4082176
_publ_section_title
;
 Annelation of Phosphole-Substituted Fischer Carbene Complexes by Alkynes
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7482
_journal_paper_doi               10.1021/om4009795
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C19 H15 O6 P W'
_chemical_formula_sum            'C19 H15 O6 P W'
_chemical_formula_weight         554.13
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 104.875(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0588(11)
_cell_length_b                   10.7193(9)
_cell_length_c                   15.8075(14)
_cell_measurement_temperature    153(2)
_cell_volume                     1974.8(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29635
_diffrn_reflns_theta_full        31.05
_diffrn_reflns_theta_max         31.05
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    5.962
_exptl_absorpt_correction_T_max  0.2514
_exptl_absorpt_correction_T_min  0.2103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.864
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.830
_refine_diff_density_min         -1.294
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         6319
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0234
_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^)+(0.0250P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0544
_reflns_number_gt                5325
_reflns_number_total             6319
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4009795_si_001.cif
_cod_data_source_block           mat158s
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4082176