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_4126929
_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            'C111 H138 N7 P Y3'
_chemical_formula_weight         1867.98
_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                104.401(6)
_cell_angle_beta                 110.072(6)
_cell_angle_gamma                90.263(7)
_cell_formula_units_Z            2
_cell_length_a                   15.401(6)
_cell_length_b                   21.019(8)
_cell_length_c                   22.180(8)
_cell_measurement_reflns_used    4625
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.39
_cell_measurement_theta_min      2.34
_cell_volume                     6500(4)
_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      296(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.1196
_diffrn_reflns_av_unetI/netI     0.3271
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            38324
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.050
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_min         1.005
_exptl_absorpt_coefficient_mu    1.379
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.434
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.954
_exptl_crystal_description       prism
_exptl_crystal_F_000             1970
_exptl_crystal_size_max          1.000
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.200
_platon_squeeze_details          ' '
_refine_diff_density_max         2.482
_refine_diff_density_min         -1.256
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1127
_refine_ls_number_reflns         22688
_refine_ls_number_restraints     281
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.2006
_refine_ls_R_factor_gt           0.1146
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.7608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2724
_refine_ls_wR_factor_ref         0.3023
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8107
_reflns_number_total             22688
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            5a.cif
_cod_data_source_block           mo_60713a
_cod_database_code               4126929
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.339
_shelx_estimated_absorpt_t_max   0.770
_shelx_res_checksum              68532
_shelx_hkl_checksum              33058