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_7107481
_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 Br I2 N'
_chemical_formula_sum            'C5 H2 Br I2 N'
_chemical_formula_weight         409.79
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 89.993(5)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   7.065(6)
_cell_length_b                   12.192(11)
_cell_length_c                   9.672(8)
_cell_measurement_reflns_used    2204
_cell_measurement_temperature    299
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.33
_cell_volume                     833.1(12)
_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 0.898
_diffrn_measured_fraction_theta_max 0.898
_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  0.0850
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5431
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.279
_exptl_absorpt_correction_T_max  0.541
_exptl_absorpt_correction_T_min  0.304
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             720.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.690
_refine_diff_density_min         -1.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.888
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     82
_refine_ls_number_reflns         1716
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0315P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1020
_reflns_number_gt                1066
_reflns_number_total             1716
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c2cc17958j.txt
_cod_data_source_block           Py345IBI
_cod_database_code               7107481