Efficient Reagent-Saving Method for the N-Terminal Labeling of Bioactive Peptides with Organometallic Carboxylic Acids by Solid-Phase Synthesis
Slootweg, Jack C.; Albada, H. Bauke; Siegmund, Daniel; Metzler-Nolte, Nils; Organometallics 35 (2016) 3192–; doi:10.1021/acs.organomet.6b00544

data_4086720
_publ_section_title
;
 Efficient Reagent-Saving Method for the N-Terminal Labeling of Bioactive
 Peptides with Organometallic Carboxylic Acids by Solid-Phase Synthesis
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              3192
_journal_paper_doi               10.1021/acs.organomet.6b00544
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C32 H27 Cl N3 O6 Re'
_chemical_formula_weight         771.21
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                92.057(3)
_cell_angle_beta                 96.839(2)
_cell_angle_gamma                101.301(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4340(2)
_cell_length_b                   10.4154(3)
_cell_length_c                   16.3142(5)
_cell_measurement_reflns_used    12878
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      3.119
_cell_volume                     1557.86(7)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford Xcalibur 2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12878
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.119
_exptl_absorpt_coefficient_mu    4.033
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_description       needle
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.570
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         5469
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0334P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0623
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4798
_reflns_number_total             5469
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00544_si_001.cif
_cod_data_source_block           Re-complex5
_cod_database_code               4086720
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.499
_shelx_estimated_absorpt_t_max   0.689
_shelx_res_checksum              38537
_shelx_hkl_checksum              79594