Reversible dioxygen binding on asymmetric dinuclear rhodium centres
Takayuki Nakajima; Miyuki Sakamoto; Sachi Kurai; Bunsho Kure; Tomoaki Tanase; Chem.Commun. 49 (2013) 5250–; doi:10.1039/c3cc41815d

data_7109351
_publ_section_title
;
 Reversible dioxygen binding on asymmetric dinuclear rhodium centres
;
_journal_name_full               Chem.Commun.
_journal_page_first              5250
_journal_paper_doi               10.1039/c3cc41815d
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C60 H64.50 Cl2 N5.50 O2 P4 Rh2'
_chemical_formula_sum            'C60 H64.5 Cl2 N5.5 O2 P4 Rh2'
_chemical_formula_weight         1295.32
_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
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                73.940(7)
_cell_angle_beta                 80.980(6)
_cell_angle_gamma                74.474(7)
_cell_formula_units_Z            2
_cell_length_a                   12.604(6)
_cell_length_b                   12.861(5)
_cell_length_c                   20.226(9)
_cell_measurement_reflns_used    9307
_cell_measurement_temperature    153
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      3.01
_cell_volume                     3024(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      153
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            35608
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.54
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1326.00
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.043
_platon_squeeze_details
;
SQUEEZE removed 17 e- at (0, 0, 0.5), corresponding to MeCN/cell or 0.5 MeCN/aymmetric unit. This molecule could not be located owing to disorder. However, this is included here in the empirical formula and calculations based on it.
;
_refine_diff_density_max         2.810
_refine_diff_density_min         -2.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     674
_refine_ls_number_reflns         13775
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1011P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1934
_reflns_number_gt                10071
_reflns_number_total             13775
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c3cc41815d.txt
_cod_data_source_block           '[Rh2Cl2(O2)(dpmppp)(MesNC)](2c)'
_cod_original_cell_volume        3023(3)
_cod_original_formula_sum        'C60 H64.50 Cl2 N5.50 O2 P4 Rh2'
_cod_database_code               7109351