Unique sodium-caged structure of a potent endothelin-1 inhibitor: crystal structure of BQ123 sodium salt, cyclo(-d-Trp-d-Asp−-Pro-d-Val-Leu-)·Na+
Doi, Mitsunobu; Ishida, Toshimasa; Katsuya, Yoshio; Mezaki, Yoshihiro; Sasaki, Masahiro; Terashima, Akira; Taniguchi, Taizo; Hasegawa, Hiroshi; Shiono, Masaaki; Chemical Communications  (2000) 743–; doi:10.1039/a909413j

data_7110804
_publ_section_title
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 Unique sodium-caged structure of a potent endothelin-1 inhibitor: crystal
 structure of BQ123 sodium salt,
 cyclo(-d-Trp-d-Asp&#x2212;-Pro-d-Val-Leu-)&#x00B7;Na+
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_journal_issue                   9
_journal_name_full               'Chemical Communications'
_journal_page_first              743
_journal_paper_doi               10.1039/a909413j
_journal_year                    2000
_chemical_compound_source        'synthesis (from BACHEM)'
_chemical_formula_moiety         '4(C31 H41 N6 O7 Na), 8(C3 H8 O), 10(H2 O)'
_chemical_formula_sum            'C148 H248 N24 Na4 O46'
_chemical_formula_weight         3191.66
_chemical_name_common            BQ123
_chemical_name_systematic
; 
 Endothelin inhibitor BQ123 Na: 
   cyclo(-D-Trp-D-Asp-Pro-D-Val-Leu-),Na
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_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.399(5)
_cell_length_b                   34.717(5)
_cell_length_c                   25.74(3)
_cell_measurement_temperature    100
_cell_volume                     22697(3)
_computing_cell_refinement       'Rigaku Process 4.0'
_computing_data_collection       'Rigaku Process 4.0'
_computing_data_reduction        'Rigaku Process 4.0'
_computing_molecular_graphics    'ORTEP-III (Burnett & Johnson 1996)'
_computing_publication_material  'PARST (Nardelli, 1983)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.780
_diffrn_measured_fraction_theta_max 0.780
_diffrn_measurement_device_type  'Rigaku RAXIS-4'
_diffrn_measurement_method       region-profit
_diffrn_radiation_monochromator  diamond
_diffrn_radiation_source         'synchrotron (SPring8)'
_diffrn_radiation_type           'double monochromated beam'
_diffrn_radiation_wavelength     0.83400
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            35804
_diffrn_reflns_theta_full        31.42
_diffrn_reflns_theta_max         31.42
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.076
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.934
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6864
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.4(3)
_refine_ls_extinction_coef       0.0116(3)
_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_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2088
_refine_ls_number_reflns         35332
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0845
_refine_ls_shift/su_max          5.873
_refine_ls_shift/su_mean         0.285
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1687P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2146
_refine_ls_wR_factor_ref         0.2241
_reflns_number_gt                31000
_reflns_number_total             35332
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            a909413jsup1.cif
_cod_data_source_block           bq
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1687P)^2^+0.0000P] 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^)+(0.1687P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        22693(24)
_cod_database_code               7110804