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_4084119
_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         'C34 H40 N4 P Tm, C7 H8'
_chemical_formula_sum            'C41 H48 N4 P Tm'
_chemical_formula_weight         796.73
_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
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_audit_creation_date             2013-12-18T16:17:12-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 92.7420(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7289(3)
_cell_length_b                   19.5591(4)
_cell_length_c                   17.0420(5)
_cell_measurement_reflns_used    7106
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1
_cell_measurement_wavelength     0.71073
_cell_volume                     3572.13(16)
_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 0.99
_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      -0.026097
_diffrn_orient_matrix_UB_12      -0.007735
_diffrn_orient_matrix_UB_13      0.054847
_diffrn_orient_matrix_UB_21      -0.088487
_diffrn_orient_matrix_UB_22      0.010123
_diffrn_orient_matrix_UB_23      -0.017225
_diffrn_orient_matrix_UB_31      -0.014014
_diffrn_orient_matrix_UB_32      -0.049514
_diffrn_orient_matrix_UB_33      -0.01209
_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  0.0541
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.99
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22234
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.99
_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
_diffrn_reflns_theta_max         27.523
_diffrn_reflns_theta_min         1.586
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    2.563
_exptl_absorpt_correction_T_max  0.632
_exptl_absorpt_correction_T_min  0.607
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.948
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       0.00007(6)
_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   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     425
_refine_ls_number_reflns         8132
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0471
_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^)+26.4470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.1027
_reflns_number_gt                5750
_reflns_number_total             8132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500607r_si_002.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 4084117--4084119.cif.'
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               4084119
_publcif_datablock.id            {1c2f0d7e-34cc-4a6d-91a6-484769e617db}