Cp*Rh-Based Heterometallic Metallarectangles: Size-Dependent Borromean Link Structures and Catalytic Acyl Transfer
Sheng-Li Huang; Yue-Jian Lin; T. S. Andy Hor; Guo-Xin Jin; Journal of the American Chemical Society 135 (2013) 8125–8128; doi:10.1021/ja402630g

data_4119840
_publ_contact_author
; 
Guo-Xin Jin
Advanced Materials Laboratory, Department of Chemistry, Fudan University, 
Shanghai 200433, P. R. China
;
_publ_contact_author_email       gxjin@fudan.edu.cn
_publ_section_title
;
 Cp*Rh-Based Heterometallic Metallarectangles: Size-Dependent Borromean
 Link Structures and Catalytic Acyl Transfer
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8125
_journal_page_last               8128
_journal_paper_doi               10.1021/ja402630g
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C73 H90 Cu2 F6 N10 O25.33 Rh4 S2'
_chemical_formula_weight         2229.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           173
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   35.098(3)
_cell_length_b                   35.098(3)
_cell_length_c                   15.8896(14)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.23
_cell_measurement_theta_min      2.19
_cell_volume                     16952(3)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0618
_diffrn_reflns_av_sigmaI/netI    0.0585
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            124948
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         0.67
_diffrn_standards_decay_%        6.30
_exptl_absorpt_coefficient_mu    1.048
_exptl_absorpt_correction_T_max  0.7439
_exptl_absorpt_correction_T_min  0.6015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             6748
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.30
_platon_squeeze_details          ' '
_refine_diff_density_max         1.172
_refine_diff_density_min         -1.721
_refine_diff_density_rms         0.162
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.022(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1140
_refine_ls_number_reflns         25826
_refine_ls_number_restraints     170
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1175P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1640
_refine_ls_wR_factor_ref         0.1788
_reflns_number_gt                19156
_reflns_number_total             25826
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja402630g_si_001_5.cif
_cod_data_source_block           6
_cod_original_cell_volume        16952(2)
_cod_database_code               4119840