Bis(phenyl)dirhodium(III) Caprolactamate: A Dinuclear Paddlewheel Complex with No Metal-Metal Bond
Jason M. Nichols; Joffrey Wolf; Peter Zavalij; Bindhu Varughese; Michael P. Doyle; Journal of the American Chemical Society 129 (2007) 3504–3505; doi:10.1021/ja070122s

data_4109239
_publ_contact_author             'Michael P. Doyle'
_publ_contact_author_email       mdoyle3@umd.edu
_publ_section_title
;
 Bis(phenyl)dirhodium(III) Caprolactamate: A Dinuclear Paddlewheel Complex
 with No Metal-Metal Bond
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3504
_journal_page_last               3505
_journal_paper_doi               10.1021/ja070122s
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C24 H44 N4 O6 Rh2, C F3 O3 S'
_chemical_formula_sum            'C25 H44 F3 N4 O9 Rh2 S'
_chemical_formula_weight         839.52
_chemical_name_common            'dirhodium caprolactamate hydrate triflate'
_chemical_name_systematic
;
Di-rhodium(II/III) tetra-caprolactamate dihydrate triflate 
;
_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 & ZCIF'
_cell_angle_alpha                90.00
_cell_angle_beta                 121.245(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.663(4)
_cell_length_b                   7.1764(13)
_cell_length_c                   21.213(4)
_cell_measurement_reflns_used    2975
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.2
_cell_volume                     3210.0(10)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'XSHEL (Bruker, 1999)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker Smart1000'
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_details      606,606,246
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      0.0450134
_diffrn_orient_matrix_UB_12      -0.0139051
_diffrn_orient_matrix_UB_13      0.0412222
_diffrn_orient_matrix_UB_21      0.0144973
_diffrn_orient_matrix_UB_22      0.0091139
_diffrn_orient_matrix_UB_23      -0.0360355
_diffrn_orient_matrix_UB_31      0.0035625
_diffrn_orient_matrix_UB_32      0.1383496
_diffrn_orient_matrix_UB_33      0.0065229
_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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19459
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.25
_diffrn_source_current           40
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0.00
_exptl_absorpt_coefficient_mu    1.165
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            dark-purple
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       plate
_exptl_crystal_F_000             1708
_exptl_crystal_id                Doyle/Nichols
_exptl_crystal_preparation       'Diethyl ether slow diffusion in CH2Cl2'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         3464
_refine_ls_number_restraints     173
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.027P)^2^+13.28P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0796
_reflns_number_gt                4172
_reflns_number_total             3464
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja070122ssi20070115_065443.cif
_cod_data_source_block           3
_cod_original_cell_volume        3209.9(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4109239
_diffrn_measurement_total_frames-ccd 1458
_diffrn_measurement_frame_width-ccd 0.3
_diffrn_detector_distance-ccd    4.958
_diffrn_measurement_frame_time-ccd 30
_diffrn_measurement_total_time-ccd 15.05
_diffrn_measurement_frame_size-ccd 512