Oxidative diamination promoted by dinuclear iodine(III) reagents.
Röben, Caren; Souto, José A; Escudero-Adán, Eduardo C; Muñiz, Kilian; Organic letters 15 (2013) 1008–1011; doi:10.1021/ol3034884

data_1556143
_publ_section_title
;
 Oxidative diamination promoted by dinuclear iodine(III) reagents.
;
_journal_issue                   5
_journal_name_full               'Organic letters'
_journal_page_first              1008
_journal_page_last               1011
_journal_paper_doi               10.1021/ol3034884
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C41 H37 Cl3 I2 N2 O9 S4'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                84.1430(10)
_cell_angle_beta                 86.0170(10)
_cell_angle_gamma                84.7420(10)
_cell_formula_units_Z            2
_cell_length_a                   9.3373(3)
_cell_length_b                   15.5995(4)
_cell_length_c                   15.8053(5)
_cell_measurement_reflns_used    9666
_cell_measurement_temperature    100(2)
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_cell_measurement_theta_min      2.19
_cell_volume                     2276.30(12)
_computing_cell_refinement       'Bruker APEX2 v2009.1-0'
_computing_data_collection       'Bruker APEX2 v2009.1-0'
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_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.738
_diffrn_measurement_device_type  'Kappa 4-axis goniometer bruker-nonius'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support
'magnetic support whith 10 micron nylon fiber cryoloop'
_diffrn_radiation_monochromator  'Multilayer Montel 200 mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
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_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34422
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_diffrn_reflns_theta_max         31.05
_diffrn_reflns_theta_min         1.76
_diffrn_source                   'rotating anode X-ray tube'
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_diffrn_source_size              '3 mm x 0.3 mm fine focus'
_diffrn_source_type              'Bruker-Nonius FR 591'
_exptl_absorpt_coefficient_mu    1.797
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_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS Version 2008/1 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.157
_refine_diff_density_min         -0.917
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_refine_ls_extinction_method     none
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_refine_ls_number_reflns         10756
_refine_ls_number_restraints     877
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+1.6193P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0820
_reflns_number_gt                8250
_reflns_number_total             10756
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol3034884_si_003.cif
_cod_data_source_block           mo_cr080_0m
_cod_depositor_comments
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The following automatic conversions were performed:

data name '_diffrn_measurement_specimen_suppport' was replaced with
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Automatic conversion script
Id: cif_correct_tags 6909 2019-04-08 15:41:33Z antanas 

The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
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Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
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_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1556143