Stepwise Synthesis of Metal-Organic Frameworks: Replacement of Structural Organic Linkers
Brandon J. Burnett; Paul M. Barron; Chunhua Hu; Wonyoung Choe; Journal of the American Chemical Society 133 (2011) 9984–9987; doi:10.1021/ja201911v

data_4106337
_publ_section_title
;
 Stepwise Synthesis of Metal-Organic Frameworks: Replacement of Structural
 Organic Linkers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9984
_journal_page_last               9987
_journal_paper_doi               10.1021/ja201911v
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C58 H34 N6 O9 Zn3'
_chemical_formula_sum            'C58 H34 N6 O9 Zn3'
_chemical_formula_weight         1155.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           129
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2a'
_symmetry_space_group_name_H-M   'P 4/n m m :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.7036(9)
_cell_length_b                   16.7036(9)
_cell_length_c                   20.765(2)
_cell_measurement_reflns_used    6713
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.98
_cell_measurement_theta_min      2.31
_cell_volume                     5793.6(7)
_computing_cell_refinement       'SAINT+ (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2005)'
_computing_data_reduction        SAINT+
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full .997
_diffrn_measured_fraction_theta_max .997
_diffrn_measurement_device_type  'Bruker SMART Apex CCD'
_diffrn_measurement_method       '\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  0.0780
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31134
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         0.98
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.645
_exptl_absorpt_correction_T_max  0.9797
_exptl_absorpt_correction_T_min  0.7038
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ' SADABS (Sheldrick, 2007)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    0.662
_exptl_crystal_description       plate
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.586
_exptl_crystal_size_mid          0.564
_exptl_crystal_size_min          0.032
_platon_squeeze_details
;
Disordered, independent solvent molecules were eliminated from the refinement 
using SQUEEZE/PLATON [Spek, A.L. (2003), J. Appl. Cryst. 36, 7-13].

R factors before data are squeezed:
_refine_ls_R_factor_all           0.1711 
_refine_ls_R_factor_gt            0.1286 
_refine_ls_wR_factor_ref          0.3939 
_refine_ls_wR_factor_gt           0.3577 
;
_refine_diff_density_max         2.247
_refine_diff_density_min         -.517
_refine_diff_density_rms         .098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2905
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0654
_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^)+(0.1137P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1600
_refine_ls_wR_factor_ref         0.1700
_reflns_number_gt                2019
_reflns_number_total             2905
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja201911v_si_002.cif
_cod_data_source_block           c8ch16sq
_cod_original_sg_symbol_H-M      'P 4/n m m'
_cod_database_code               4106337