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_4084118
_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         'C38 H56 N2 P2 Tm'
_chemical_formula_sum            'C38 H56 N2 P2 Tm'
_chemical_formula_weight         771.71
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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             2014-02-04T19:33:30-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 101.7340(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6690(10)
_cell_length_b                   16.1780(10)
_cell_length_c                   21.3200(10)
_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                     3603.0(4)
_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 0.934
_diffrn_measured_fraction_theta_max 0.962
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.934
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13960
_diffrn_reflns_point_group_measured_fraction_full 0.934
_diffrn_reflns_point_group_measured_fraction_max 0.962
_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        25.24
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.026
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    2.579
_exptl_absorpt_correction_T_max  0.814
_exptl_absorpt_correction_T_min  0.544
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1588
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.389
_refine_diff_density_min         -1.335
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     404
_refine_ls_number_reflns         6097
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0875P)^2^+14.6562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.132
_refine_ls_wR_factor_ref         0.1406
_reflns_number_gt                5597
_reflns_number_total             6097
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500607r_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4084117--4084119.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4084118
_publcif_datablock.id            {c368b9c8-b59b-4b23-bb0c-9fd36d9ed81e}