Conformational Determinants of Agonist versus Antagonist Properties of [d-Pen2,d-Pen5]Enkephalin (DPDPE) Analogs at Opioid Receptors. Comparison of X-ray Crystallographic Structure, Solution 1H NMR Data, and Molecular Dynamic Simulations of [l-Ala3]DPDPE and [d-Ala3]DPDPE
Nathan Collins; Judith L. Flippen-Anderson; Ronald C. Haaseth; Jeffery R. Deschamps; Clifford George; Katalin Kövér; Victor J. Hruby; Journal of the American Chemical Society 118 (1996) 2143–2152; doi:10.1021/ja9531081

data_4117112
_publ_section_title
;
 Conformational Determinants of Agonist versus Antagonist Properties of
 [d-Pen2,d-Pen5]Enkephalin (DPDPE) Analogs at Opioid Receptors. Comparison
 of X-ray Crystallographic Structure, Solution 1H NMR Data, and Molecular
 Dynamic Simulations of [l-Ala3]DPDPE and [d-Ala3]DPDPE
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2143
_journal_page_last               2152
_journal_paper_doi               10.1021/ja9531081
_journal_volume                  118
_journal_year                    1996
_chemical_formula_moiety         '4(C31 H41 N5 O7 S2) . 20.5 H2 O'
_chemical_formula_sum            'C124 H202 N20 O48.5 S8'
_chemical_formula_weight         3083.3
_chemical_name_common            'L-Ala DPDPE'
_chemical_name_systematic
; 
 Tyr-cyclo[D-Pen-Ala-Phe-D-Pen]
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 129.07(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   36.356(13)
_cell_length_b                   19.737(4)
_cell_length_c                   28.161(11)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      49.0
_cell_measurement_theta_min      35.3
_cell_volume                     15688(10)
_computing_cell_refinement       SHELXTL
_computing_data_collection       SHELXTL
_computing_data_reduction        SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1995)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      243(2)
_diffrn_measurement_device       'Siemens R3'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_sigmaI/netI    0.1243
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9382
_diffrn_reflns_theta_max         50.55
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        'random +/- 2.5%'
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.76
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       rods
_exptl_crystal_F_000             6764
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(5)
_refine_ls_extinction_coef       0.00023(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.098
_refine_ls_goodness_of_fit_obs   1.157
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1789
_refine_ls_number_reflns         8449
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.119
_refine_ls_restrained_S_obs      1.150
_refine_ls_R_factor_all          0.1451
_refine_ls_R_factor_obs          0.0983
_refine_ls_shift/esd_max         -0.429
_refine_ls_shift/esd_mean        0.029
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1241P)^2^+155.8387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2865
_refine_ls_wR_factor_obs         0.2315
_reflns_number_observed          5770
_reflns_number_total             8470
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9531081_1.cif
_cod_data_source_block           hr02e
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1241P)^2^+155.8387P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1241P)^2^+155.8387P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        15688.4(89)
_cod_database_code               4117112
_cod_database_fobs_code          4117112