Synthesis and Characterization of 1,1′-Diphosphaplumbocenes: Oxidative Ligand Transfer Reactions with Divalent Thulium Complexes
Jaroschik, Florian; Momin, Aurélien; Martinez, Agathe; Harakat, Dominique; Ricard, Louis; Le Goff, Xavier Frédéric; Nocton, Grégory; Organometallics 35 (2016) 2032–; doi:10.1021/acs.organomet.6b00313

data_4086501
_publ_section_title
;
 Synthesis and Characterization of 1,1&#x2032;-Diphosphaplumbocenes:
 Oxidative Ligand Transfer Reactions with Divalent Thulium Complexes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2032
_journal_paper_doi               10.1021/acs.organomet.6b00313
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C42 H72 P3 Tm'
_chemical_formula_sum            'C42 H72 P3 Tm'
_chemical_formula_weight         838.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.993(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.540(1)
_cell_length_b                   11.751(1)
_cell_length_c                   18.521(1)
_cell_measurement_reflns_used    5256
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     4143.8(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29795
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.85
_exptl_absorpt_coefficient_mu    2.284
_exptl_absorpt_correction_T_max  0.8384
_exptl_absorpt_correction_T_min  0.5474
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'yellowish green'
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.069
_refine_diff_density_min         -1.298
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         11783
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+9.5495P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0750
_reflns_number_gt                10328
_reflns_number_total             11783
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00313_si_002.cif
_cod_data_source_block           amx554
_cod_depositor_comments
'Adding full bibliography for 4086501--4086502.cif.'
_cod_original_sg_symbol_H-M      'P21/c     '
_cod_database_code               4086501