Copper-Catalyzed Aminoalkynylation of Alkenes with Hypervalent Iodine Reagents
Shen, Kun; Wang, Qiu; Chem. Sci.  (2017) –; doi:10.1039/C7SC03420B

data_1547681
_publ_section_title
;
 Copper-Catalyzed Aminoalkynylation of Alkenes with Hypervalent Iodine
 Reagents
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC03420B
_journal_year                    2017
_chemical_formula_moiety         'C27 H27 N O4, 0.5(C4 H8 O2)'
_chemical_formula_sum            'C29 H31 N2 O5'
_chemical_formula_weight         473.54
_chemical_name_common            'SK-V-211-2 minor'
_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_update_record
;
2017-08-05 deposited with the CCDC.
2017-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                65.705(3)
_cell_angle_beta                 73.172(4)
_cell_angle_gamma                89.520(4)
_cell_formula_units_Z            4
_cell_length_a                   10.3428(7)
_cell_length_b                   16.0861(11)
_cell_length_c                   17.3663(12)
_cell_measurement_reflns_used    9798
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      30.4612
_cell_measurement_theta_min      2.3280
_cell_volume                     2500.3(3)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection       'Bruker Instrument Service v2013.12.0.0'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 786)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker-Nonius X8 Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            98492
_diffrn_reflns_theta_full        30.59
_diffrn_reflns_theta_max         30.59
_diffrn_reflns_theta_min         1.48
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.352
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.485
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         15311
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0616
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+2.1946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1663
_refine_ls_wR_factor_ref         0.1771
_reflns_number_gt                11862
_reflns_number_total             15311
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc03420b2.cif
_cod_data_source_block           rds625
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

2019-08-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C27 H27 N O4), C4 H8 O2'
_cod_original_formula_sum        'C58 H62 N2 O10'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     947.09
_cod_database_code               1547681
_shelx_res_checksum              2126