Single molecule magnets with m-fluorobenzoate and difluoromethylacetate as polar ligands.
Hoshino, Norihisa; Shiga, Takuya; Oshio, Hiroki; Akutagawa, Tomoyuki; Dalton transactions (Cambridge, England : 2003) 42 (2013) 4377–4385; doi:10.1039/c2dt32498a

data_7021083
_publ_section_title
;
 Single molecule magnets with m-fluorobenzoate and difluoromethylacetate
 as polar ligands.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4377
_journal_page_last               4385
_journal_paper_doi               10.1039/c2dt32498a
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C32 H24 F32 Mn12 O48, 4(H2O), 2(C H2 Cl2)'
_chemical_formula_sum            'C34 H36 Cl4 F32 Mn12 O52'
_chemical_formula_weight         2685.71
_chemical_name_systematic
;
?
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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            2
_cell_length_a                   17.7242(12)
_cell_length_b                   17.7242(12)
_cell_length_c                   12.6228(16)
_cell_measurement_reflns_used    8004
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.30
_cell_volume                     3965.4(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11085
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    2.154
_exptl_absorpt_correction_T_max  0.7671
_exptl_absorpt_correction_T_min  0.5218
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
The asymmetric unit contained disordered CH2Cl2 solvent molecules and could
not be modeled properly. Analyses in lower symmetric space groups resulted
in vain. Thus PLATON/SQUEEZE promgram was used to evaluate the solvent
disorder area and remove its contribution to the overall intensity data.
;
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4427
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+8.8825P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0877
_reflns_number_gt                4312
_reflns_number_total             4427
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt32498a.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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_database_code               7021083