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_4126931
_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            'C104 H130 Lu3 N6 P S4'
_chemical_formula_weight         2148.25
_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                79.553(3)
_cell_angle_beta                 73.921(3)
_cell_angle_gamma                76.979(3)
_cell_formula_units_Z            2
_cell_length_a                   15.272(4)
_cell_length_b                   15.635(4)
_cell_length_c                   26.536(6)
_cell_measurement_reflns_used    4605
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.43
_cell_measurement_theta_min      2.22
_cell_volume                     5884(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0411
_diffrn_reflns_av_unetI/netI     0.1122
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            29013
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.048
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_min         1.348
_exptl_absorpt_coefficient_mu    2.622
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       block
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_platon_squeeze_details          ' '
_refine_diff_density_max         1.554
_refine_diff_density_min         -1.130
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1090
_refine_ls_number_reflns         20368
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0472P)^2^+0.4593P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1348
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11701
_reflns_number_total             20368
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            9b.cif
_cod_data_source_block           a50315b
_cod_original_cell_volume        5884(2)
_cod_database_code               4126931
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.650
_shelx_estimated_absorpt_t_max   0.779
_shelx_res_checksum              26690
_shelx_hkl_checksum              67889