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_4329182
_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         'C28 H8 N6 O8 Zn2'
_chemical_formula_sum            'C28 H8 N6 O8 Zn2'
_chemical_formula_weight         687.14
_chemical_name_common            DMOF-1-dcppy-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                   15.1370(18)
_cell_length_b                   15.1370(18)
_cell_length_c                   9.6187(12)
_cell_measurement_reflns_used    4607
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.17
_cell_measurement_theta_min      2.51
_cell_volume                     2203.9(5)
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0647
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6352
_diffrn_reflns_theta_full        25.26
_diffrn_reflns_theta_max         25.26
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_T_max  0.9458
_exptl_absorpt_correction_T_min  0.9202
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.518
_exptl_crystal_description       block
_exptl_crystal_F_000             342
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
Squeeze found 292 electrons that can be accounted to 6 EtOAc molecules. The
structure was not refined as anisotropy because when it is refined as anisotropy
some atoms have N.P.D. The nitrogen atom on the dcppy ligand was refined to be
disorder over 4 positions which has an 25% occupancy each.
;
_refine_diff_density_max         10.711
_refine_diff_density_min         -8.324
_refine_diff_density_rms         0.363
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.919
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     24
_refine_ls_number_reflns         1201
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.919
_refine_ls_R_factor_all          0.2279
_refine_ls_R_factor_gt           0.2131
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.007
_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          0.5297
_refine_ls_wR_factor_ref         0.5750
_reflns_number_gt                988
_reflns_number_total             1201
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202683s_si_003_4.cif
_cod_data_source_block           DMOF-1-dcppy
_cod_database_code               4329182