Exceptionally Stable, Hollow Tubular Metal-Organic Architectures: Synthesis, Characterization, and Solid-State Transformation Study
Cheng-Yong Su; Andrea M. Goforth; Mark D. Smith; P. J. Pellechia; Hans-Conrad zur Loye; Journal of the American Chemical Society 126 (2004) 3576–3586; doi:10.1021/ja039022m

data_4112353
_publ_section_title
;
 Exceptionally Stable, Hollow Tubular Metal-Organic Architectures:
 Synthesis, Characterization, and Solid-State Transformation Study
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3576
_journal_page_last               3586
_journal_paper_doi               10.1021/ja039022m
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C2 H3 F N4 O0.86 Zn'
_chemical_formula_weight         181.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                120.00
_cell_formula_units_Z            18
_cell_length_a                   18.5486(7)
_cell_length_b                   18.5486(7)
_cell_length_c                   9.8538(7)
_cell_measurement_reflns_used    3826
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.294
_cell_measurement_theta_min      2.196
_cell_volume                     2936.0(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0189
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5619
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    3.705
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6919
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_description       needle
_exptl_crystal_F_000             1599
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0233
_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^)+(0.0437P)^2^+2.3706P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0647
_reflns_number_gt                760
_reflns_number_total             815
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja039022msi20031007_110549.cif
_cod_data_source_block           st0315bs
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4112353