Diastereoselective Formation of Metallamacrocyclic (Arene)RuII and Cp*RhIII Complexes
Marie-Line Lehaire; Rosario Scopelliti; Lorenz Herdeis; Kurt Polborn; Peter Mayer; Kay Severin; Inorganic Chemistry 43 (2004) 1609–1617; doi:10.1021/ic035328i

data_4310682
_publ_contact_author_address
;
Institut de Chimie Mol\'eculaire et Biologique
\'Ecole Polytechnique F\'ed\'erale de Lausanne
1015 Lausanne
Switzerland
;
_publ_contact_author_email       kay.severin@epfl.ch
_publ_contact_author_fax         '+41 21 693 9305'
_publ_contact_author_name        'Kay Severin'
_publ_contact_author_phone       '+41 21 693 9302'
_publ_section_title
;
 Diastereoselective Formation of Metallamacrocyclic (Arene)RuII and
 Cp*RhIII Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1609
_journal_page_last               1617
_journal_paper_doi               10.1021/ic035328i
_journal_volume                  43
_journal_year                    2004
_chemical_compound_source        'provided by K. Severin'
_chemical_formula_moiety         '2(Rh, C10H15, O3 N C6 H3, H2 O), Cl3 H C'
_chemical_formula_sum            'C33 H41 Cl3 N2 O8 Rh2'
_chemical_formula_weight         905.856
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_author_name               'Mayer, P.'
_audit_block_code                Rh_Cp*_NO3C6_H2O_en018_severin
_audit_creation_date             17-Aug-00
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_cell_angle_alpha                107.7288(14)
_cell_angle_beta                 90.3147(13)
_cell_angle_gamma                109.5758(8)
_cell_formula_units_Z            2
_cell_length_a                   9.65790(20)
_cell_length_b                   11.81110(20)
_cell_length_c                   17.68810(29)
_cell_measurement_reflns_used    11380
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     1797.74(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics
;ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid
 Plot Program for Crystal Structure Illustrations, Oak Ridge National
 Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ.
 Glasgow) used --- SCHAKAL (E. Keller, University of  Freiburg (Breisgau),
 Germany, 1995).
;
_computing_publication_material
;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version).
--- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses).
;
_computing_structure_refinement
'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)'
_computing_structure_solution
'SIR97 (Cascarano et al.,Acta Crystallogr., Sect A, 1996, C79)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_collimation    0.6_mm
_diffrn_radiation_monochromator  'vertically mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0611
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16373
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.57
_diffrn_source_current           75_mA
_diffrn_source_power             4.1_kW
_diffrn_source_type              'rotating anode'
_diffrn_source_voltage           55_kV
_exptl_absorpt_coefficient_mu    1.192
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.67347(6)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.682
_refine_diff_density_min         -1.141
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         7977
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.1076
_reflns_number_gt                6378
_reflns_number_total             7977
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035328isi20031118_025229_2.cif
_cod_data_source_block           16
_cod_original_cell_volume        1797.738(60)
_cod_database_code               4310682