Synthesis, Structure, Assembly, and Modulation of the CO2 Adsorption Properties of a Zinc-Adeninate Macrocycle
Jihyun An; Richard P. Fiorella; Steven J. Geib; Nathaniel L. Rosi; Journal of the American Chemical Society 131 (2009) 8401–8403; doi:10.1021/ja901869m

data_4104571
_publ_contact_author_address
;Department of Chemistry
University of Pittsburgh
219 Parkman Ave. 
Pittsburgh, PA 15260
USA
;
_publ_contact_author_email       nrosi@pitt.edu
_publ_contact_author_name        'Nathaniel L. Rosi'
_publ_contact_author_phone       412-624-3987
_publ_section_title
;
 Synthesis, Structure, Assembly, and Modulation of the CO2 Adsorption
 Properties of a Zinc-Adeninate Macrocycle
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8401
_journal_page_last               8403
_journal_paper_doi               10.1021/ja901869m
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C78 H90 N42 O12 Zn6'
_chemical_formula_weight         2200.14
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :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            3
_cell_length_a                   17.780(3)
_cell_length_b                   17.780(3)
_cell_length_c                   33.531(7)
_cell_measurement_reflns_used    769
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      17.18
_cell_measurement_theta_min      2.29
_cell_volume                     9180(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0979
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            22999
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.80
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker Smart Apex CCD'
_exptl_absorpt_coefficient_mu    1.220
_exptl_absorpt_correction_T_max  .737
_exptl_absorpt_correction_T_min  .687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker Sadabs'
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_F_000             3384
_exptl_crystal_recrystallization_method
'slow evaporation from pyridine and dimethylformamide'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         3.227
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.222
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3418
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.222
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0716
_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^)+(0.1176P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2064
_refine_ls_wR_factor_ref         0.2233
_reflns_number_gt                2465
_reflns_number_total             3418
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja901869m_si_002.cif
_cod_data_source_block           hexa_3_4
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4104571