Interpenetrated (8,3)-c and (10,3)-b Metal‒Organic Frameworks Based on {FeIII3} and {FeIII2CoII} Pivalate Spin Clusters
Botezat, Olga; van Leusen, Jan; Kravtsov, Victor Ch.; Filippova, Irina G.; Hauser, Jürg; Speldrich, Manfred; Hermann, Raphaël P.; Krämer, Karl W.; Liu, Shi-Xia; Decurtins, Silvio; Kögerler, Paul; Baca, Svetlana G.; Crystal Growth & Design 14 (2014) 4721–; doi:10.1021/cg5008236

data_4511760
_publ_section_title
;
 Interpenetrated (8,3)-c and (10,3)-b Metal--Organic Frameworks Based on
 {FeIII3} and {FeIII2CoII} Pivalate Spin Clusters
;
_journal_issue                   9
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4721
_journal_paper_doi               10.1021/cg5008236
_journal_volume                  14
_journal_year                    2014
_chemical_formula_sum            'C91.5 H169 Cl3 Fe6 N6 O44'
_chemical_formula_weight         2498.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           192
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6 2c'
_symmetry_space_group_name_H-M   'P 6/m c c'
_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                120.00
_cell_formula_units_Z            8
_cell_length_a                   38.8452(8)
_cell_length_b                   38.8452(8)
_cell_length_c                   24.8241(7)
_cell_measurement_reflns_used    8057
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.3507
_cell_measurement_theta_min      2.8877
_cell_volume                     32439.9(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9914
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1256
_diffrn_reflns_av_sigmaI/netI    0.0902
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            69846
_diffrn_reflns_theta_full        18.84
_diffrn_reflns_theta_max         18.84
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_T_max  0.9055
_exptl_absorpt_correction_T_min  0.8785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.023
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prizm
_exptl_crystal_F_000             10552
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
;
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         4390
_refine_ls_number_restraints     708
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1390
_refine_ls_R_factor_gt           0.0849
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1470P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2254
_refine_ls_wR_factor_ref         0.2464
_reflns_number_gt                2230
_reflns_number_total             4390
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5008236_si_002.cif
_cod_data_source_block           v_49_oh29_corr
_cod_depositor_comments
'Adding full bibliography for 4511759--4511760.cif.'
_cod_original_cell_volume        32439.8(13)
_cod_original_sg_symbol_H-M      P6/mcc
_cod_original_formula_sum        'C91.50 H169 Cl3 Fe6 N6 O44'
_cod_database_code               4511760