Synthesis and Characterization of Cationic Rhodium Peroxo Complexes
Cipot-Wechsler, Judy; Covelli, Danielle; Praetorius, Jeremy M.; Hearns, Nigel; Zenkina, Olena V.; Keske, Eric C.; Wang, Ruiyao; Kennepohl, Pierre; Crudden, Cathleen M.; Organometallics 31 (2012) 7306–; doi:10.1021/om300766x

data_4079488
_publ_section_title
;
 Synthesis and Characterization of Cationic Rhodium Peroxo Complexes
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              7306
_journal_paper_doi               10.1021/om300766x
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C47 H55 F3 N6 O5 Rh S'
_chemical_formula_weight         975.94
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2012-08-30 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.251(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.344(3)
_cell_length_b                   8.6387(8)
_cell_length_c                   33.322(3)
_cell_measurement_reflns_used    9713
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.16
_cell_measurement_theta_min      2.44
_cell_volume                     9271.4(15)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0468
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            59833
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.23
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.477
_exptl_absorpt_correction_T_max  0.9538
_exptl_absorpt_correction_T_min  0.8900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4056
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
Difference electron density maps revealed the presence of a disordered 
triflate in the asymmetrical unit, which were ultimately modeled through the
use of the SQUEEZE subroutine of the PLATON software suite. PLATON 
Reference: P. v.d. Sluis & A.L. Spek. Acta Cryst. (1990), A46, 194. 
Totally 8 voids per lattice were found. Each void comprises a 
total volume of about 151 A3 and contributing a total of 88 to 90 electrons. 
The void was thus assigned to a triflate, which 
contributes 74 electrons, and ocuppy about 160 A3 in space. 
;
_refine_diff_density_max         3.945
_refine_diff_density_min         -2.644
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         9126
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0927
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+243.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2139
_refine_ls_wR_factor_ref         0.2160
_reflns_number_gt                8468
_reflns_number_total             9126
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300766x_si_002.cif
_cod_data_source_block           cc121a
_cod_original_cell_volume        9271.5(15)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4079488