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_4079487
_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            'C44 H56 Cl1.1 N4 O2.3 Rh'
_chemical_formula_weight         819.63
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 100.914(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   33.0114(13)
_cell_length_b                   10.8616(5)
_cell_length_c                   23.8287(9)
_cell_measurement_reflns_used    6078
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.21
_cell_volume                     8389.4(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0453
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            27123
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.518
_exptl_absorpt_correction_T_max  0.9597
_exptl_absorpt_correction_T_min  0.8601
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3441
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         8196
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0404P)^2^+14.8166P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.1039
_reflns_number_gt                6172
_reflns_number_total             8196
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300766x_si_002.cif
_cod_data_source_block           cc89
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C44 H56 Cl1.10 N4 O2.30 Rh'
_cod_database_code               4079487