Single-Atom Ligand Changes Affect Breathing in an Extended Metal-Organic Framework
Phuong V. Dau; Min Kim; Sergio J. Garibay; Frédéric H. L. Münch; Curtis E. Moore; Seth M. Cohen; Inorganic Chemistry 51 (2012) 5671–5676; doi:10.1021/ic202683s

data_4329181
_publ_section_title
;
 Single-Atom Ligand Changes Affect Breathing in an Extended Metal-Organic
 Framework
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5671
_journal_page_last               5676
_journal_paper_doi               10.1021/ic202683s
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C36 H16 N2 O8 Zn2'
_chemical_formula_sum            'C36 H16 N2 O8 Zn2'
_chemical_formula_weight         734.87
_chemical_name_common            DMOF-1-bpdc-6EtOAc
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           123
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4 2'
_symmetry_space_group_name_H-M   'P 4/m m 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            1
_cell_length_a                   15.210(3)
_cell_length_b                   15.210(3)
_cell_length_c                   9.6282(19)
_cell_measurement_reflns_used    2761
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.29
_cell_measurement_theta_min      2.50
_cell_volume                     2227.4(8)
_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      200(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            872
_diffrn_reflns_theta_full        22.30
_diffrn_reflns_theta_max         22.30
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.561
_exptl_absorpt_correction_T_max  0.9461
_exptl_absorpt_correction_T_min  0.9206
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.553
_exptl_crystal_description       block
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
Squeeze found 288 electrons that can be accounted to 6 ethyl acetate molecules.
No hydrogen atoms was added to C6 and C7 because of the highly disorders of 
dabco ligands. The value of sine(theta_max)/wavelength is less than 0.550 due 
to the quality of the crystal. Since the single X-ray structure information 
was to show the overall similar framework of DMOF-1-bpdc to the parent DMOF, 
attempt to collect another another structure to improve the value of 
sine(the_max)/wavelength is unnecessary.
;
_refine_diff_density_max         1.195
_refine_diff_density_min         -1.422
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     51
_refine_ls_number_reflns         872
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0655
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1930
_refine_ls_wR_factor_ref         0.1989
_reflns_number_gt                774
_reflns_number_total             872
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202683s_si_003_3.cif
_cod_data_source_block           DMOF-1-bpdc
_cod_original_cell_volume        2227.5(7)
_cod_database_code               4329181