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_4086502
_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         'C28 H48 P2 Pb'
_chemical_formula_sum            'C28 H48 P2 Pb'
_chemical_formula_weight         653.79
_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                 125.591(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.845(1)
_cell_length_b                   15.665(1)
_cell_length_c                   19.616(1)
_cell_measurement_reflns_used    7237
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     2959.8(4)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) & COLLECT'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        'DENZO & COLLECT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15003
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    5.821
_exptl_absorpt_correction_T_max  0.4561
_exptl_absorpt_correction_T_min  0.3608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.122
_refine_diff_density_min         -0.940
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       0.00098(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         8582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0146P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.0503
_reflns_number_gt                6674
_reflns_number_total             8582
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00313_si_002.cif
_cod_data_source_block           pbp2tbu
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 4086501--4086502.cif.
;
_cod_original_cell_volume        2959.8(3)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4086502