Single Crystal to Single Crystal Transformation and Hydrogen-Atom Transfer upon Oxidation of a Cerium Coordination Compound
Ursula J. Williams; Brian D. Mahoney; Andrew J. Lewis; Patrick T. DeGregorio; Patrick J. Carroll; Eric J. Schelter; Inorganic Chemistry 52 (2013) 4142–4144; doi:10.1021/ic4001973

data_4334514
_publ_section_title
;
 Single Crystal to Single Crystal Transformation and Hydrogen-Atom
 Transfer upon Oxidation of a Cerium Coordination Compound
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4142
_journal_page_last               4144
_journal_paper_doi               10.1021/ic4001973
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C52 H60 Ce N8'
_chemical_formula_weight         937.20
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.435(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.524(4)
_cell_length_b                   18.559(3)
_cell_length_c                   16.309(3)
_cell_measurement_temperature    143(1)
_cell_volume                     5590.0(18)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      143(1)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0095
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            72063
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.851
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.241
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         6396
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.241
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0233
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+6.9858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0748
_reflns_number_gt                6123
_reflns_number_total             6396
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4001973_si_002_1.cif
_cod_data_source_block           UP465
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_database_code               4334514