Hydrogen-bonded DeUG x DAN heterocomplex: structure and stability and a scalable synthesis of DeUG with reactive functionality.
Kuykendall, Darrell W.; Anderson, Cyrus A.; Zimmerman, Steven C.; Organic letters 11 (2009) 61–64; doi:10.1021/ol802344w

data_1503720
_publ_contact_author
; 
Scott R. Wilson 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_section_title
;
 Hydrogen-bonded DeUG x DAN heterocomplex: structure and stability and a
 scalable synthesis of DeUG with reactive functionality.
;
_journal_issue                   1
_journal_name_full               'Organic letters'
_journal_page_first              61
_journal_page_last               64
_journal_paper_doi               10.1021/ol802344w
_journal_volume                  11
_journal_year                    2009
_chemical_formula_moiety         'C22 H35 N5 O2, C22 H32 N4 O2'
_chemical_formula_sum            'C44 H67 N9 O4'
_chemical_formula_weight         786.07
_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
_audit_update_record
; 
2006-11-1    text and data added, mr 
;
_cell_angle_alpha                105.078(8)
_cell_angle_beta                 101.351(8)
_cell_angle_gamma                96.175(8)
_cell_formula_units_Z            2
_cell_length_a                   10.773(6)
_cell_length_b                   11.224(6)
_cell_length_c                   19.641(10)
_cell_measurement_reflns_used    913
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      38.203
_cell_measurement_theta_min      4.916
_cell_volume                     2216(2)
_computing_cell_refinement       'SAINT V6.22 (Bruker, 2001)'
_computing_data_collection       'SMART V5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT V6.22 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL V6.12 (Bruker, 2001)'
_computing_publication_material  'XCIF (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2001)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2001)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       'Siemens Platform/CCD'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_radiation_wavelength_id  g53nas
_diffrn_reflns_av_R_equivalents  0.0969
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_diffrn_reflns_limit_h_min       -12
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_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
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_diffrn_reflns_theta_max         25.43
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        25.0
_diffrn_standards_interval_time  244
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_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  0.9863
_exptl_absorpt_correction_T_min  0.9626
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP (Bruker, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabular
_exptl_crystal_F_000             852
_exptl_crystal_id                g53nas
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (2 -2 1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.192
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         8030
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.1883
_refine_ls_R_factor_gt           0.0656
_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^)+(0.0665P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1853
_reflns_number_gt                3157
_reflns_number_total             8030
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol802344w_si_001.cif
_cod_data_source_block           g53ntas
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2217(2)
_cod_database_code               1503720