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_7051542
_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_sum            'C68 H72 O6 P2 Y2'
_chemical_formula_weight         1225.02
_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                86.89(3)
_cell_angle_beta                 75.64(3)
_cell_angle_gamma                70.68(3)
_cell_formula_units_Z            2
_cell_length_a                   12.513(3)
_cell_length_b                   14.455(3)
_cell_length_c                   19.023(4)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    200(2)
_cell_volume                     3144.1(14)
_computing_data_collection       STOE-X-AREA
_computing_molecular_graphics    XP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  STOE-IPDSII
_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  0.1327
_diffrn_reflns_av_sigmaI/netI    0.1414
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40601
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    1.936
_exptl_absorpt_correction_type   'mean imaging plate intensity method'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.949
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.899
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         11055
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.897
_refine_ls_R_factor_all          0.1193
_refine_ls_R_factor_gt           0.0624
_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^)+(0.0682P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1511
_reflns_number_gt                6310
_reflns_number_total             11055
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b514439f.txt
_cod_data_source_block           ks394
_cod_original_cell_volume        3144.4(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7051542