Control of cerium oxidation state through metal complex secondary structures
Levin, Jessica R.; Dorfner, Walter L.; Carroll, Patrick J.; Schelter, Eric J.; Chem. Sci. 6 (2015) 6925–; doi:10.1039/C5SC02607E

data_1529391
_publ_section_title
;
 Control of cerium oxidation state through metal complex secondary
 structures
;
_journal_issue                   12
_journal_name_full               'Chem. Sci.'
_journal_page_first              6925
_journal_paper_doi               10.1039/C5SC02607E
_journal_volume                  6
_journal_year                    2015
_chemical_formula_sum            'C83 H75 Ce K5 N15'
_chemical_formula_weight         1618.20
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Heat-sensitive, Oxygen-sensitive'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-06-03 deposited with the CCDC.
2015-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                93.849(5)
_cell_angle_beta                 101.333(5)
_cell_angle_gamma                107.292(5)
_cell_formula_units_Z            2
_cell_length_a                   15.2003(12)
_cell_length_b                   15.4668(12)
_cell_length_c                   18.0353(15)
_cell_measurement_temperature    143(1)
_cell_volume                     3933.7(6)
_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 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0544
_diffrn_reflns_av_sigmaI/netI    0.0581
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            95153
_diffrn_reflns_theta_full        27.61
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1662
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Pyridine hexanes'
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.264
_refine_diff_density_min         -2.044
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     968
_refine_ls_number_reflns         17890
_refine_ls_number_restraints     456
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+6.9251P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1570
_reflns_number_gt                13252
_reflns_number_total             17890
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc02607e2.cif
_cod_data_source_block           CMPD3(UP4331)
_cod_depositor_comments
'Adding full bibliography for 1529389--1529391.cif.'
_cod_original_cell_volume        3933.7(5)
_cod_original_sg_symbol_H-M      'P -1       '
_cod_database_code               1529391