Multiple One-Electron Transfers in Bipyridine Complexes of Bis(phospholyl) Thulium
Jacquot, Léa; Xémard, Mathieu; Clavaguéra, Carine; Nocton, Grégory; Organometallics 33 (2014) 4100–; doi:10.1021/om500607r

data_4084117
_publ_section_title
;
 Multiple One-Electron Transfers in Bipyridine Complexes of
 Bis(phospholyl) Thulium
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4100
_journal_paper_doi               10.1021/om500607r
_journal_volume                  33
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C42 H64 P4 Tm'
_chemical_formula_sum            'C42 H64 P4 Tm'
_chemical_formula_weight         861.74
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2014-02-04T16:14:01-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 108.009(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1927(5)
_cell_length_b                   11.5425(3)
_cell_length_c                   20.4504(6)
_cell_measurement_reflns_used    8445
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1
_cell_measurement_wavelength     0.71073
_cell_volume                     4084.0(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.043051
_diffrn_orient_matrix_UB_12      0.035221
_diffrn_orient_matrix_UB_13      -0.037712
_diffrn_orient_matrix_UB_21      0.038069
_diffrn_orient_matrix_UB_22      0.049805
_diffrn_orient_matrix_UB_23      -0.01327
_diffrn_orient_matrix_UB_31      0.006172
_diffrn_orient_matrix_UB_32      -0.06152
_diffrn_orient_matrix_UB_33      -0.032334
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            25885
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_reduction_process
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         2.052
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    2.357
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1780
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.316
_refine_diff_density_min         -1.314
_refine_diff_density_rms         0.254
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     424
_refine_ls_number_reflns         9286
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+28.9827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1405
_refine_ls_wR_factor_ref         0.1569
_reflns_number_gt                7093
_reflns_number_total             9286
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500607r_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 4084117--4084119.cif.'
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               4084117