An Unprecedented Reaction Mode of phosphorus in phosphinidene rare-earth complex: a joint experimental-theoretical study.
Tian, Haiwen; Hong, Jianquan; Wang, Kai; Del Rosal, Iker; Maron, Laurent; Zhou, Xigeng; Zhang, Lixin; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b11032

data_4126932
_publ_section_title
;
 An Unprecedented Reaction Mode of phosphorus in phosphinidene rare-earth
 complex: a joint experimental-theoretical study.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b11032
_journal_year                    2017
_chemical_formula_sum            'C109 H131 N6 P Y3'
_chemical_formula_weight         1822.89
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                77.644(5)
_cell_angle_beta                 74.669(5)
_cell_angle_gamma                69.197(5)
_cell_formula_units_Z            2
_cell_length_a                   16.134(7)
_cell_length_b                   16.740(7)
_cell_length_c                   23.731(10)
_cell_measurement_reflns_used    4196
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      25.49
_cell_measurement_theta_min      2.19
_cell_volume                     5727(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_unetI/netI     0.2185
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            27383
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.050
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_min         1.380
_exptl_absorpt_coefficient_mu    1.563
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.474
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.057
_exptl_crystal_description       sheet
_exptl_crystal_F_000             1918
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.150
_platon_squeeze_details
;
;
_refine_diff_density_max         0.811
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1074
_refine_ls_number_reflns         19680
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.1781
_refine_ls_R_factor_gt           0.0949
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.3387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2323
_refine_ls_wR_factor_ref         0.2488
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8217
_reflns_number_total             19680
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            2a.cif
_cod_data_source_block           a60402b
_cod_database_code               4126932
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.651
_shelx_estimated_absorpt_t_max   0.799
_shelx_res_checksum              53842
_shelx_hkl_checksum              73966