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_4126928
_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            'C43 H49 N2 S2 Y'
_chemical_formula_weight         746.87
_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                66.952(2)
_cell_angle_beta                 81.691(2)
_cell_angle_gamma                67.608(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8274(15)
_cell_length_b                   13.2630(18)
_cell_length_c                   15.854(2)
_cell_measurement_reflns_used    2100
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      22.10
_cell_measurement_theta_min      2.33
_cell_volume                     2115.9(5)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0422
_diffrn_reflns_av_unetI/netI     0.0884
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12896
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.048
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_min         1.396
_exptl_absorpt_coefficient_mu    1.506
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       sheet
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_platon_squeeze_details
;
;
_refine_diff_density_max         0.796
_refine_diff_density_min         -1.246
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         7386
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0673
_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^)+(0.1500P)^2^+0.1300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1943
_refine_ls_wR_factor_ref         0.2510
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5044
_reflns_number_total             7386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            7a.cif
_cod_data_source_block           mo_50520d
_cod_database_code               4126928
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.753
_shelx_estimated_absorpt_t_max   0.929
_shelx_res_checksum              10589
_shelx_hkl_checksum              21674