η5‒η1Switch in Divalent Phosphaytterbocene Complexes with Neutral Iminophosphoranyl Pincer Ligands: Solid-State Structures and Solution NMR1JYb‒PCoupling Constants
Cheisson, Thibault; Auffrant, Audrey; Nocton, Grégory; Organometallics 34 (2015) 5470–; doi:10.1021/acs.organomet.5b00814

data_4088051
_publ_section_title
;
 \h5--\h1Switch in Divalent Phosphaytterbocene Complexes with Neutral
 Iminophosphoranyl Pincer Ligands: Solid-State Structures and Solution
 NMR1JYb--PCoupling Constants
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5470
_journal_paper_doi               10.1021/acs.organomet.5b00814
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C26 H34 N2 P2 Yb'
_chemical_formula_sum            'C26 H34 N2 P2 Yb'
_chemical_formula_weight         609.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 109.475(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.281(1)
_cell_length_b                   10.192(1)
_cell_length_c                   17.485(1)
_cell_measurement_reflns_used    6762
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     2567.4(3)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) & COLLECT'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        'DENZO & COLLECT'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22300
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         30.012
_diffrn_reflns_theta_min         2.947
_exptl_absorpt_coefficient_mu    3.783
_exptl_absorpt_correction_T_max  1.30604
_exptl_absorpt_correction_T_min  0.854704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   DENZO/SCALEPACK
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.216
_refine_diff_density_min         -1.046
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         7422
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0541
_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^)+18.6534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.1042
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5756
_reflns_number_total             7422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00814_si_002.cif
_cod_data_source_block           tc382
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4088051
_shelx_estimated_absorpt_t_min   0.417
_shelx_estimated_absorpt_t_max   0.963
_shelxl_version_number           2013-4
_shelx_res_checksum              64250
_shelx_hkl_checksum              52132