Synthesis and characterization of a zinc metal‒organic framework with chiral nano-pores
Shen, Lingjuan; Gray, Danielle; Masel, Richard I.; Girolami, Gregory S.; CrystEngComm 14 (2012) 5145–; doi:10.1039/c2ce25780g

data_7208399
_publ_section_title
;
 Synthesis and characterization of a zinc metal--organic framework with
 chiral nano-pores
;
_journal_issue                   16
_journal_name_full               CrystEngComm
_journal_page_first              5145
_journal_paper_doi               10.1039/c2ce25780g
_journal_volume                  14
_journal_year                    2012
_chemical_absolute_configuration rmad
_chemical_formula_moiety
;
C26 H14 N4 O12 Zn3, 2(C5 H11 N O)
;
_chemical_formula_sum            'C36 H36 N6 O14 Zn3'
_chemical_formula_weight         972.82
_chemical_name_systematic
;
?
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
?
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1751(3)
_cell_length_b                   15.1751(3)
_cell_length_c                   22.5604(8)
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.74
_cell_measurement_theta_min      4.89
_cell_volume                     5195.3(2)
_computing_cell_refinement       'SAINT V7.68A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2010.11-3 (Bruker, 2010)'
_computing_data_reduction
;
SAINT V7.68A, XPREP V2005/2, SADABS V2007/4, TWINABS V2007/5
(Bruker, 2005 & 2007)
;
_computing_molecular_graphics
;
SHELXTL V6.12 (Bruker, 2005), CrystalMaker v2.1.3 (CrystalMaker, 1994)
;
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Bruker prospector/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'Mx optics'
_diffrn_radiation_source         'Imus microfocus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_wavelength_id  92asq
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_sigmaI/netI    0.0191
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            57131
_diffrn_reflns_theta_full        67.73
_diffrn_reflns_theta_max         67.73
_diffrn_reflns_theta_min         4.12
_exptl_absorpt_coefficient_mu    2.111
_exptl_absorpt_correction_T_max  0.9322
_exptl_absorpt_correction_T_min  0.8488
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1984
_exptl_crystal_id                92asq
_exptl_crystal_preparation
;
The data crystal was mounted using oil (Parantone-N, Exxon) to a
glass fiber.
;
_exptl_crystal_size_max          0.164
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
The solvent accessible voids contain diethylformamide (DEF), water or
formic acid. For the sake of the absorption coefficient, it
was assumed that the voids contain only DEF. One DEF has 56 electrons,
which is equivalent to approximately 8.5 DEF/void. Z=4 so the amount of
DEF/assymetric unit is approximately 2.1 DEF. The amount of DEF reported
in the moiety, calculated into the molecular weight, the density and
the absorption coefficient was 2 molecules of DEF.
;
_refine_diff_density_max         1.109
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 'Flack (1983), 1955 Friedels'
_refine_ls_abs_structure_Flack   0.50(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         4672
_refine_ls_number_restraints     503
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0754P)^2^+3.7584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1178
_reflns_number_gt                4593
_reflns_number_total             4672
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25780g.txt
_cod_data_source_block           92asq
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_Hall     'P 4abw 2nw '
_cod_original_sg_symbol_H-M      'P4(1)2(1)2 '
_cod_database_code               7208399