Symmetric Heteropolynuclear Ti(IV)/Cu(I) Complexes Exhibiting Stepwise Electrochemical Reductions to Ti(III) Species
Pierre Le Gendre; Virginie Comte; Marie-Joëlle Ondel-Eymin; Claude Moïse; Eveline Pousson; Philippe Richard; Yves Mugnier; Daniel Fortin; René T. Boeré; Pierre D. Harvey; Inorganic Chemistry 48 (2009) 3095–3103; doi:10.1021/ic8023869

data_4301874
_publ_contact_author_address
;
lseo, facult\'e des sciences Mirande
9 All\'ee Alain Savary 
21000 dijon,
france
;
_publ_contact_author_email       prichard@u-bourgogne.fr
_publ_contact_author_fax         +33-0380396098
_publ_contact_author_name        'richard, philippe'
_publ_contact_author_phone       +33-0380396079
_publ_section_title
;
Symmetric Heteropolynuclear Ti(IV)/Cu(I) Complexes Exhibiting Stepwise
Electrochemical Reductions to Ti(III) Species
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3095
_journal_page_last               3103
_journal_paper_doi               10.1021/ic8023869
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C44 H38 Cl5 Cu P2 Ti2, 3(C H2 Cl2)'
_chemical_formula_sum            'C47 H44 Cl11 Cu P2 Ti2'
_chemical_formula_weight         1220.05
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                76.1490(10)
_cell_angle_beta                 80.1560(10)
_cell_angle_gamma                69.9410(10)
_cell_formula_units_Z            2
_cell_length_a                   10.57500(10)
_cell_length_b                   15.2335(2)
_cell_length_c                   17.1021(3)
_cell_measurement_reflns_used    10514
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     2500.72(6)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius,1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPIII (Burnett, 1996)'
_computing_publication_material  'SHELXL97 and WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare, 1993)'
_diffrn_ambient_temperature      115(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Kappa CCD'
_diffrn_measurement_method       '\f scans (\k = 0) + additional \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20106
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.06
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.419
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.000
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         11430
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+0.5200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0758
_reflns_number_gt                8792
_reflns_number_total             11430
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8023869_si_001_3.cif
_cod_data_source_block           3
_cod_database_code               4301874