Tetranuclear Manganese(II) Complexes of Thiacalixarene Macrocycles with Trigonal Prismatic Six-Coordinate Geometries: Synthesis, Structure, and Magnetic Properties
Cédric Desroches; Guillaume Pilet; Serguei A. Borshch; Stéphane Parola; Dominique Luneau; Inorganic Chemistry 44 (2005) 9112–9120; doi:10.1021/ic050507g

data_4310037
_publ_contact_author_address
;
Cristallographie et Ingenierie Moleculaire
Laboratoire des Multimateriaux et Interfaces - UMR 5615
Universite Claude Bernard Lyon 1
Bat. Jules Raulin
43 Bd du 11 Novembre 1918
69622 Villeurbanne Cedex
FRANCE
;
_publ_contact_author_email       dominique.luneau@univ-lyon1.fr
_publ_contact_author_fax         '(+33)4 72 43 11 60'
_publ_contact_author_name        'Dominique Luneau'
_publ_contact_author_phone       '(+33)4 72 44 82 20'
_publ_section_title
;
Tetranuclear Manganese(II) Complexes of Thiacalixarene Macrocycles with
Trigonal Prismatic Six-Coordinate Geometries: Synthesis, Structure, and
Magnetic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9112
_journal_page_last               9120
_journal_paper_doi               10.1021/ic050507g
_journal_volume                  44
_journal_year                    2005
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C20.00 H20.5 Mn1.00 O2.25 S2.00 '
_chemical_formula_sum            'C80 H82 Mn4 O9 S8'
_chemical_formula_weight         1663.8
_chemical_name_systematic
;
?
;
_space_group_IT_number           71
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2 2'
_symmetry_space_group_name_H-M   'I m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             05-10-03
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.213(5)
_cell_length_b                   19.037(5)
_cell_length_c                   29.159(5)
_cell_measurement_reflns_used    6426
_cell_measurement_temperature    293
_cell_measurement_theta_max      28
_cell_measurement_theta_min      1
_cell_volume                     10110(4)
_computing_cell_refinement
;
 Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
 COLLECT (Nonius BV, 1997)
;
_computing_data_reduction
;
 Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics
;
 CAMERON (Watkin et al 1996)
;
_computing_publication_material
;
 CRYSTALS (Watkin et al 2003)
;
_computing_structure_refinement
;
 CRYSTALS (Watkin et al 2003)
;
_computing_structure_solution
;
 SIR97 (Altomare et al, 1999)
;
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
;
Nonius Kappa CCD
;
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.05
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            12025
_diffrn_reflns_theta_full        27.886
_diffrn_reflns_theta_max         27.886
_diffrn_reflns_theta_min         1.277
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_T_max  0.00
_exptl_absorpt_correction_T_min  0.00
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            ' ? '
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_description       ' cubic '
_exptl_crystal_F_000             2799.500
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.13
_refine_diff_density_min         -0.83
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0476
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         2235
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.2283
_refine_ls_R_factor_gt           0.0992
_refine_ls_shift/su_max          0.003635
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
 Method = Robust Weighting (Prince, 1982)
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
 A~i~ are:
 1.55 1.25 1.13
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1853
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.0962
_reflns_limit_h_max              23
_reflns_limit_h_min              0
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              38
_reflns_limit_l_min              0
_reflns_number_gt                2235
_reflns_number_total             6507
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ic050507gsi20050406_124748_1.cif
_cod_data_source_block           CRYSTALS_cif
_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 
;
_cod_original_sg_symbol_H-M      'I m m m '
_cod_original_formula_sum        ' C80.00 H82.00 Mn4.00 O9.00 S8.00 '
_cod_database_code               4310037