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_4310685
_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_formula_moiety         'C57 H57 N3 O6 Ru3, C5 H12, 2(C H Cl3)'
_chemical_formula_sum            'C64 H71 Cl6 N3 O6 Ru3'
_chemical_formula_weight         1494.15
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.7004(17)
_cell_length_b                   18.2764(17)
_cell_length_c                   27.586(2)
_cell_measurement_reflns_used    7756
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      22.0588
_cell_measurement_theta_min      2.11655
_cell_volume                     12453.3(17)
_computing_cell_refinement       'Oxford Diffraction CrysAlis RED'
_computing_data_collection       'Oxford Diffraction CrysAlis CCD'
_computing_data_reduction        'Oxford Diffraction CrysAlis RED'
_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      140(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Oxford Diffraction KM4 Sapphire CCD'
_diffrn_measurement_method       'phi and omega 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  0.0604
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            73291
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.50
_exptl_absorpt_coefficient_mu    1.029
_exptl_absorpt_correction_T_max  0.8150
_exptl_absorpt_correction_T_min  0.4410
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
; 
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) 
;
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             6064
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.761
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         10420
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0859P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1529
_reflns_number_gt                7365
_reflns_number_total             10420
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035328isi20031118_025229_5.cif
_cod_data_source_block           19
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_original_cell_volume        12453.1(17)
_cod_database_code               4310685