Formation of unusual molecular rectangles and squares containing low spin and high spin Co(ii) and Fe(ii) centers
Shuvaev, Konstantin V.; Dawe, Louise N.; Thompson, Laurence K.; Dalton Transactions 39 (2010) 4768–; doi:10.1039/b915595c

data_7024345
_publ_section_title
;
 Formation of unusual molecular rectangles and squares containing low spin
 and high spin Co(ii) and Fe(ii) centers
;
_journal_issue                   20
_journal_name_full               'Dalton Transactions'
_journal_page_first              4768
_journal_paper_doi               10.1039/b915595c
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety
'2(C15 H14 N6 S), 2(C15 H15 N6 S), 4Co, 2(C F3 O3 S), 13(H2 O)'
_chemical_formula_sum            'C62 H84 Co4 F6 N24 O19 S6'
_chemical_formula_weight         2011.58
_chemical_name_systematic
;
?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 103.404(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.950(3)
_cell_length_b                   27.769(6)
_cell_length_c                   13.903(3)
_cell_measurement_reflns_used    17601
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.9251
_cell_measurement_theta_min      2.5033
_cell_volume                     4487.9(18)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_publication_material  'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'graphite-Rigaku SHINE'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0818
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            20154
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    0.954
_exptl_absorpt_correction_T_max  0.9660
_exptl_absorpt_correction_T_min  0.8974
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(T. Higashi, 2000)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2068
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
The Platon Squeeze procedure was applied to recover 422 electrons per
unit cell in one void (total volume 1557 ^A^3); that is 211 electrons
per formula unit. One very badly disordered triflate anion, and several
disordered solvent lattice water molecules were present prior to the
application of Squeeze, however, despite numerous attempts at modeling,
a satisfactory point atom model could not be achieved. The application
of Squeeze gave a good improvement in the data statistics and allowed for
a full anisotropic refinement of the structure.
PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13
;
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         9406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0692
_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^)+(0.1078P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1877
_refine_ls_wR_factor_ref         0.2044
_reflns_number_gt                6308
_reflns_number_total             9406
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b915595c.txt
_cod_data_source_block           Compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        4487.9(16)
_cod_database_code               7024345