Synthesis and molecular structures of the first phosphoranylidene complexes of rare earth metals
Rufanov, Konstantin A.; Müller, Bernd H.; Spannenberg, Anke; Rosenthal, Uwe; New Journal of Chemistry 30 (2006) 29–; doi:10.1039/b514439f

data_7051541
_publ_section_title
;
 Synthesis and molecular structures of the first phosphoranylidene
 complexes of rare earth metals
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              29
_journal_paper_doi               10.1039/b514439f
_journal_volume                  30
_journal_year                    2006
_chemical_formula_moiety         'C26 H23 O P'
_chemical_formula_sum            'C26 H23 O P'
_chemical_formula_weight         382.41
_chemical_name_common            Triphenylphosphonium-ortho-methoxybenzylide
_chemical_name_systematic
;
Triphenylphosphonium-ortho-methoxybenzylide
;
_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                73.76(2)
_cell_angle_beta                 85.61(2)
_cell_angle_gamma                89.94(2)
_cell_formula_units_Z            2
_cell_length_a                   9.7457(18)
_cell_length_b                   10.0458(18)
_cell_length_c                   10.715(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      3.0
_cell_volume                     1004.0(3)
_computing_cell_refinement       'IPDS2.87 (Stoe & Cie, 1997)'
_computing_data_collection       'IPDS2.87 (Stoe & Cie, 1997)'
_computing_data_reduction        'IPDS2.87 (Stoe & Cie, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Stoe IPDS diffractometer'
_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  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6420
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    0.151
_exptl_absorpt_correction_T_max  0.9881
_exptl_absorpt_correction_T_min  0.8942
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.009(3)
_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   0.934
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         3401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.934
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0553P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                2577
_reflns_number_total             3401
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b514439f.txt
_cod_data_source_block           ruf7
_cod_database_code               7051541