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_4088047
_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         'C43 H37 N3 P2'
_chemical_formula_sum            'C43 H37 N3 P2'
_chemical_formula_weight         657.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 106.105(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1526(10)
_cell_length_b                   13.8286(10)
_cell_length_c                   18.801(1)
_cell_measurement_reflns_used    7482
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     3535.2(4)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0702
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20794
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.946
_exptl_absorpt_coefficient_mu    0.158
_exptl_absorpt_correction_T_max  1.0693
_exptl_absorpt_correction_T_min  0.932394
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   DENZO/SCALEPACK
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 1974 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.829
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6060
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.829
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+20.3206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1149
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.945
_reflns_Friedel_fraction_max     0.945
_reflns_number_gt                5120
_reflns_number_total             6060
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00814_si_002.cif
_cod_data_source_block           tcl1
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4088047
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.963
_shelx_estimated_absorpt_t_max   0.994
_shelx_res_checksum              40939
_shelx_hkl_checksum              42585