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_4109237
_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         'C36 H50 N4 O4 Rh2, 2(C H2 Cl2)'
_chemical_formula_sum            'C38 H54 Cl4 N4 O4 Rh2'
_chemical_formula_weight         978.47
_chemical_name_common            'bis-phenyl dirhodium caprolactamate'
_chemical_name_systematic
;
Bis-phenyl di-rhodium(III) tetra-caprolactamate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           'SHELXL-97 & ZCIF'
_cell_angle_alpha                78.8840(10)
_cell_angle_beta                 74.4100(10)
_cell_angle_gamma                73.1860(10)
_cell_formula_units_Z            2
_cell_length_a                   10.9770(3)
_cell_length_b                   13.1258(4)
_cell_length_c                   16.0022(5)
_cell_measurement_reflns_used    7880
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      29.5
_cell_measurement_theta_min      2.2
_cell_volume                     2109.24(11)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      606,606,606,50,1206
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0550261
_diffrn_orient_matrix_UB_12      0.0549557
_diffrn_orient_matrix_UB_13      0.0393341
_diffrn_orient_matrix_UB_21      0.0205641
_diffrn_orient_matrix_UB_22      0.0584020
_diffrn_orient_matrix_UB_23      -0.0475247
_diffrn_orient_matrix_UB_31      -0.0780843
_diffrn_orient_matrix_UB_32      0.0018714
_diffrn_orient_matrix_UB_33      -0.0216797
_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  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27474
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.63
_diffrn_source_current           20
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0.14
_exptl_absorpt_coefficient_mu    1.078
_exptl_absorpt_correction_T_max  0.806
_exptl_absorpt_correction_T_min  0.685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    not_measure
_exptl_crystal_description       prism
_exptl_crystal_F_000             1000
_exptl_crystal_id                Doyle/
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.584
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.072
_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     527
_refine_ls_number_reflns         9583
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.02P)^2^+3.237P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0687
_reflns_number_gt                8323
_reflns_number_total             9583
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja070122ssi20070115_065321.cif
_cod_data_source_block           1
_cod_original_cell_volume        2109.25(11)
_cod_database_code               4109237
_diffrn_measurement_total_frames-ccd 3074
_diffrn_measurement_frame_width-ccd 0.3
_diffrn_detector_distance-ccd    4.958
_diffrn_measurement_frame_time-ccd 13
_diffrn_measurement_total_time-ccd 17.21
_diffrn_measurement_frame_size-ccd 512