Total synthesis of COPD biomarker desmosine that crosslinks elastin
Toyonobu Usuki; Haruka Yamada; Takahiro Hayashi; Hiroto Yanuma; Yohei Koseki; Noriyuki Suzuki; Yoshiro Masuyama; Yong Lin; Chem.Commun. 48 (2012) 3233–; doi:10.1039/c2cc17958j

data_7107480
_publ_section_title
;
 Total synthesis of COPD biomarker desmosine that crosslinks elastin
;
_journal_name_full               Chem.Commun.
_journal_page_first              3233
_journal_paper_doi               10.1039/c2cc17958j
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C5 H2 I3 N'
_chemical_formula_sum            'C5 H2 I3 N'
_chemical_formula_weight         456.79
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 129.4130(8)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   18.560(6)
_cell_length_b                   9.955(3)
_cell_length_c                   11.987(4)
_cell_measurement_reflns_used    2534
_cell_measurement_temperature    299
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      2.49
_cell_volume                     1711.1(9)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      299
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6176
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.883
_exptl_absorpt_correction_T_max  0.580
_exptl_absorpt_correction_T_min  0.339
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1584.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.750
_refine_diff_density_min         -1.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     82
_refine_ls_number_reflns         1913
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0268P)^2^+12.1220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                1568
_reflns_number_total             1913
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c2cc17958j.txt
_cod_data_source_block           Py345I
_cod_database_code               7107480