An Fe-based MOF constructed from paddle-wheel and rod-shaped SBUs involved in situ generated acetate
Li, Yun-Wu; Zhao, Jiong-Peng; Wang, Li-Fu; Bu, Xian-He; CrystEngComm 13 (2011) 6002–; doi:10.1039/c1ce05470h

data_7215391
_publ_section_title
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 An Fe-based MOF constructed from paddle-wheel and rod-shaped SBUs
 involved in situ generated acetate
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              6002
_journal_paper_doi               10.1039/c1ce05470h
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C41 H40 Fe5 N3 O24'
_chemical_formula_weight         1238.01
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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                 102.27(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   33.747(7)
_cell_length_b                   12.808(3)
_cell_length_c                   14.155(3)
_cell_measurement_temperature    293(2)
_cell_volume                     5978(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_av_sigmaI/netI    0.0625
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30780
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    1.257
_exptl_absorpt_correction_T_max  0.7872
_exptl_absorpt_correction_T_min  0.7198
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2516
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;

In order to subtract the contribution from the disordered solvent molecules,
the SQUEEZE command was applied, which gave a new HKL file.
There is 0 residual electron in four voids per unit cell.
This residual electron density show that there is no orther solvent molecule.
So SQUEEZE removed none of solvent molecule per formula unit.
This value calculated based upon volume/count_electrons analysis,
combining with elemental analyses, and TG analyses.
See ref. O.V. Dolomanov, D. B. Cordes, N. R. Champness, A. J. Blake,
L. R. Hanton, G. B. Jameson, M. Schroder and C. Wilson. Chem. Commun.,
2004, 642.
;
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         6841
_refine_ls_number_restraints     361
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0717
_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^)+(0.0892P)^2^+39.7320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1679
_refine_ls_wR_factor_ref         0.1829
_reflns_number_gt                5224
_reflns_number_total             6841
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce05470h.txt
_cod_data_source_block           x
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        5979(2)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7215391