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_7024344
_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
'C60 H58 Co4 N24 O4, 2 (C F3 O3 S), 5 (C H4 O)'
_chemical_formula_sum            'C67 H78 Co4 F6 N24 O15 S2'
_chemical_formula_weight         1873.35
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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                 103.532(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.230(9)
_cell_length_b                   11.985(4)
_cell_length_c                   27.967(10)
_cell_measurement_reflns_used    16625
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.6790
_cell_measurement_theta_min      2.5307
_cell_volume                     8222(5)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0634
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            53299
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    0.934
_exptl_absorpt_correction_T_max  0.9686
_exptl_absorpt_correction_T_min  0.8975
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(T. Higashi, 2000)'
_exptl_crystal_colour            'Dark Red'
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3848
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
The Platon Squeeze procedure was applied to recover 412 electrons per
unit cell in two voids (total volume 1972 ^A^3); that is 103 electrons
per formula unit. Disordered solvent lattice methanol molecules were
present prior to the application of Squeeze, however, 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         1.680
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         8511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0679
_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^)+(0.0951P)^2^+26.2140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1853
_refine_ls_wR_factor_ref         0.1931
_reflns_number_gt                7695
_reflns_number_total             8511
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b915595c.txt
_cod_data_source_block           Compound1
_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 
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_cod_database_code               7024344