A permanently porous van der Waals solid by using phosphonate monoester linkers in a metal organic framework.
Simon S. Iremonger; Junmei Liang; Ramanathan Vaidhyanathan; George K. H. Shimizu; Chem.Commun. 47 (2011) 4430–; doi:10.1039/c0cc04779a

data_7106212
_publ_section_title
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 A permanently porous van der Waals solid by using phosphonate monoester
 linkers in a metal organic framework.
;
_journal_name_full               Chem.Commun.
_journal_page_first              4430
_journal_paper_doi               10.1039/c0cc04779a
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C11 H17 O6 P2 Zn'
_chemical_formula_sum            'C11 H16 O6 P2 Zn'
_chemical_formula_weight         371.55
_chemical_name_common            Zinc-1,4-benzenediphosphonatodiethylester
_chemical_name_systematic
;
Zinc-1,4-benzenediphosphonatodiethylester
;
_space_group_IT_number           72
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2 2c'
_symmetry_space_group_name_H-M   'I b a m'
_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            8
_cell_length_a                   15.729(3)
_cell_length_b                   23.170(5)
_cell_length_c                   9.7372(19)
_cell_measurement_reflns_used    1254
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.7
_cell_measurement_theta_min      2.6
_cell_volume                     3548.6(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'HKL Denzo and Scalepack (1997)'
_computing_molecular_graphics    'HKL Denzo and Scalepack (1997)'
_computing_publication_material  'Diamond 3.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius Kappa with APEX II CCD detector'
_diffrn_measurement_method       CCD
_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  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2878
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    1.581
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS;Universitat Gottingen,1997'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod-shaped
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
A SQUEEZE analysis on compound 1, indicated an electron count per
unit cell of 2, suggesting that there is no residual solvent in the pore.
However the fact that the analytical measurements(TGA) shows solvent
loss seems to suggest that the electron densities in the channels are not
visible to the x-ray. This could mean that the electron densities in the
voids are highly diffused.
;
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1612
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0609
_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^)+(0.0743P)^2^+54.7577P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1556
_refine_ls_wR_factor_ref         0.1694
_reflns_number_gt                1241
_reflns_number_total             1612
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc04779a.txt
_cod_data_source_block           squeezed
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      Ibam
_cod_database_code               7106212