Electronic Effects in 12-Metallacrown-3 Complexes. A Theoretical and Experimental Study
Marie-Line Lehaire; Axel Schulz; Rosario Scopelliti; Kay Severin; Inorganic Chemistry 42 (2003) 3576–3581; doi:10.1021/ic034042a

data_4313717
_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
;
 Electronic Effects in 12-Metallacrown-3 Complexes. A Theoretical and
 Experimental Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3576
_journal_page_last               3581
_journal_paper_doi               10.1021/ic034042a
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety
'C45 H48 Cl4 Li N3 O6 Ru3, C H Cl3, 1.5 (H2 O)'
_chemical_formula_sum            'C46 H52 Cl7 Li N3 O7.5 Ru3'
_chemical_formula_weight         1325.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 106.455(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.041(3)
_cell_length_b                   16.332(3)
_cell_length_c                   33.167(4)
_cell_measurement_reflns_used    3476
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      22.8345
_cell_measurement_theta_min      1.6295
_cell_volume                     10411(3)
_computing_cell_refinement       'Oxford Diffraction CrysAlis RED'
_computing_data_collection       'marresearch, mar345'
_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 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'mar345 IPDS'
_diffrn_measurement_method
'60 images with deltaphi = 3 deg. and exp. time = 180 sec.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            29623
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.29
_exptl_absorpt_coefficient_mu    1.270
_exptl_absorpt_correction_T_max  0.3870
_exptl_absorpt_correction_T_min  0.0230
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
; 
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             5304
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.068
_refine_diff_density_min         -1.934
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       0.00023(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         8639
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0652
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0824P)^2^+49.5240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1727
_refine_ls_wR_factor_ref         0.1917
_reflns_number_gt                6697
_reflns_number_total             8639
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034042asi20030116_034304_2.cif
_cod_data_source_block           3_x_LiCl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        'C46 H52 Cl7 Li N3 O7.50 Ru3'
_cod_database_code               4313717