Amino acid bioconjugation via iClick reaction of an oxanorbornadiene-masked alkyne with a MnI(bpy)(CO)3-coordinated azide
Lucas Henry; Christoph Schneider; Benedict Mutzel; Peter V. Simpson; Christoph Nagel; Katharina Fucke; Ulrich Schatzschneider; Chem.Commun. 50 (2014) 15692–; doi:10.1039/C4cc07892F

data_7116102
_publ_section_title
;
 Amino acid bioconjugation via iClick reaction of an
 oxanorbornadiene-masked alkyne with a MnI(bpy)(CO)3-coordinated azide
;
_journal_name_full               Chem.Commun.
_journal_page_first              15692
_journal_paper_doi               10.1039/C4cc07892F
_journal_volume                  50
_journal_year                    2014
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C29 H24 F3 Mn N6 O6'
_chemical_formula_sum            'C29 H24 F3 Mn N6 O6'
_chemical_formula_weight         664.48
_chemical_name_systematic
'(OC-6-33)-tricarbonyl(4,4'-dimethyl-2,2'-bipyridine)(4-oxo-DL-phenylalanyl-5-trifluoromethyl-2H-1,2,3-triazolate-N2) manganese(I)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-09-22
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.280(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.2447(8)
_cell_length_b                   15.2085(12)
_cell_length_c                   10.6362(9)
_cell_measurement_reflns_used    6654
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      2.35
_cell_volume                     1479.8(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.9926
_diffrn_measured_fraction_theta_max 0.9926
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18131
_diffrn_reflns_theta_full        25.9978
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.93
_diffrn_source                   'sealed tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.518
_exptl_absorpt_correction_T_max  0.9418
_exptl_absorpt_correction_T_min  0.8034
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1022 before and 0.0557 after correction. The Ratio of minimum to maximum transmission is 0.8393. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.4911
_exptl_crystal_description       block
_exptl_crystal_F_000             681.0834
_exptl_crystal_recrystallization_method
'crystalls were obtained by slow diffusion of hexane in DCM solution'
_exptl_crystal_size_max          0.645
_exptl_crystal_size_mid          0.406
_exptl_crystal_size_min          0.382
_refine_diff_density_max         0.3420
_refine_diff_density_min         -0.2685
_refine_diff_density_rms         0.0560
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.000(12)
_refine_ls_d_res_high            0.8107
_refine_ls_d_res_low             10.5253
_refine_ls_goodness_of_fit_ref   1.0369
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    41
_refine_ls_number_parameters     408
_refine_ls_number_reflns         5767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0369
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0372P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0750
_reflns_Friedel_coverage         0.985
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              18
_reflns_limit_k_min              -18
_reflns_limit_l_max              13
_reflns_limit_l_min              -13
_reflns_number_gt                5342
_reflns_number_total             5767
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c4cc07892f2.cif
_cod_data_source_block
'[Mn(triazolateCO-Phe-OCH3,CF3)(bpyCH3,CH3)(CO)3]'
_cod_database_code               7116102
_olex2_refinement_description
;
;
_olex2_submission_special_instructions 'No special instructions were received'