Removal of Metal−Metal Bonding in a Dimetallic Paddlewheel Complex: Molecular and Electronic Structure of Bis(phenyl) Dirhodium(III) Carboxamidate Compounds
Wolf, Joffrey; Poli, Rinaldo; Xie, Jian-Hua; Nichols, Jason; Xi, Bin; Zavalij, Peter; Doyle, Michael P.; Organometallics 27 (2008) 5836–; doi:10.1021/om800631b

data_4072163
_publ_section_title
;
 Removal of Metal&#x2212;Metal Bonding in a Dimetallic Paddlewheel
 Complex: Molecular and Electronic Structure of Bis(phenyl) Dirhodium(III)
 Carboxamidate Compounds
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5836
_journal_paper_doi               10.1021/om800631b
_journal_volume                  27
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C30 H34 N6 O4 Rh2, 0.704(C H2 Cl2), B F4'
_chemical_formula_sum            'C30.7 H35.4 B Cl1.4 F4 N6 O4 Rh2'
_chemical_formula_weight         894.71
_chemical_name_systematic
; 
Tetrakis-\m-(pyrrolidinato)-bis(benzonitrile)dirhodium(II,III) 
tetrafluoroborate 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 97.983(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.1512(14)
_cell_length_b                   15.890(3)
_cell_length_c                   13.803(2)
_cell_measurement_reflns_used    4948
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      28.8
_cell_measurement_theta_min      2.5
_cell_volume                     1770.5(5)
_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      220(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker Smart1000'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      606,606,606,1206
_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      0.0326884
_diffrn_orient_matrix_UB_12      0.0069183
_diffrn_orient_matrix_UB_13      0.0720992
_diffrn_orient_matrix_UB_21      -0.0122657
_diffrn_orient_matrix_UB_22      -0.0619982
_diffrn_orient_matrix_UB_23      0.0091687
_diffrn_orient_matrix_UB_31      0.1188522
_diffrn_orient_matrix_UB_32      -0.0082678
_diffrn_orient_matrix_UB_33      -0.0082950
_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  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18292
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.56
_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_standards_decay_%        1.21
_exptl_absorpt_coefficient_mu    1.103
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_density_method    not-measur
_exptl_crystal_description       plate
_exptl_crystal_F_000             897
_exptl_crystal_id
'Doyle/Wolfe WJ491: Et2O, pentane, MeCN, H2O, solvent=Ph-CN?'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.867
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details '(Flack, 1983)'
_refine_ls_abs_structure_Flack   0.43(5)
_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     454
_refine_ls_number_reflns         8029
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0351
_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^)+(0.014P)^2^+4.065P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0798
_reflns_Friedel_coverage         0.912
_reflns_number_gt                7058
_reflns_number_total             8029
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800631b_si_002.cif
_cod_data_source_block           2a'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1770.6(5)
_cod_original_sg_symbol_H-M      P21
_cod_original_formula_sum        'C30.70 H35.40 B Cl1.40 F4 N6 O4 Rh2'
_cod_database_code               4072163
_diffrn_measurement_total_frames-ccd 3024
_diffrn_measurement_frame_width-ccd 0.3
_diffrn_detector_distance-ccd    4.939
_diffrn_measurement_frame_time-ccd 23
_diffrn_measurement_total_time-ccd 25.33
_diffrn_measurement_frame_size-ccd 512