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_4329180
_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         'C34 H20 N6 O8 Zn2'
_chemical_formula_sum            'C34 H20 N6 O8 Zn2'
_chemical_formula_weight         771.30
_chemical_name_common            BMOF-1-dcppy-10.2EtOAc
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                76.892(2)
_cell_angle_beta                 86.550(2)
_cell_angle_gamma                83.446(2)
_cell_formula_units_Z            2
_cell_length_a                   14.020(2)
_cell_length_b                   15.082(2)
_cell_length_c                   15.121(2)
_cell_measurement_reflns_used    3399
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.57
_cell_measurement_theta_min      2.41
_cell_volume                     3091.7(7)
_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 0.996
_diffrn_measured_fraction_theta_max 0.984
_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  0.0625
_diffrn_reflns_av_sigmaI/netI    0.0727
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37147
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.21
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    0.809
_exptl_absorpt_correction_T_max  0.9607
_exptl_absorpt_correction_T_min  0.9235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.828
_exptl_crystal_description       plate
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
Squeeze found 489 electrons that can be accounted for ~10.2 EtOAc
molecules. The nitrogen atom on the dcppy ligand was refined as 
disorder over two position and split was used to determine the occupancy
of each position. The structure was not refined as anisotropy because when
it is refined as anisotropy some atoms have N.P.D.
;
_refine_diff_density_max         3.366
_refine_diff_density_min         -2.611
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         10962
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1220
_refine_ls_R_factor_gt           0.1007
_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^)+(0.1938P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2654
_refine_ls_wR_factor_ref         0.2853
_reflns_number_gt                7100
_reflns_number_total             10962
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202683s_si_003_2.cif
_cod_data_source_block           BMOF-1-dcppy
_cod_original_cell_volume        3091.8(9)
_cod_database_code               4329180