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_4088054
_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         'C59 H97 N3 P4 Yb'
_chemical_formula_sum            'C59 H97 N3 P4 Yb'
_chemical_formula_weight         1145.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 96.486(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.994(1)
_cell_length_b                   34.291(1)
_cell_length_c                   27.1533(9)
_cell_measurement_reflns_used    19839
_cell_measurement_temperature    150.0(1)
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_cell_measurement_theta_min      0.998
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_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) & COLLECT'
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_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
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_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         30.032
_diffrn_reflns_theta_min         2.716
_exptl_absorpt_coefficient_mu    1.299
_exptl_absorpt_correction_T_max  1.39934
_exptl_absorpt_correction_T_min  0.793739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   DENZO/SCALEPACK
_exptl_crystal_colour            'Dark Purple'
_exptl_crystal_density_diffrn    0.968
_exptl_crystal_description       Block
_exptl_crystal_F_000             4816
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.092
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         22675
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0250P)^2^+60.6719P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1119
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16878
_reflns_number_total             22675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00814_si_002.cif
_cod_data_source_block           tc467
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4088054
_shelx_estimated_absorpt_t_min   0.563
_shelx_estimated_absorpt_t_max   0.781
_shelxl_version_number           2014/6
_shelx_res_checksum              60645
_shelx_hkl_checksum              79171
_shelx_fab_checksum              90889