Pd-Catalyzed allylic C-H activation to seven-membered <i>N</i>,<i>O</i>-heterocycles.
Velasco-Rubio, Álvaro; Varela, Jesús A; Saá, Carlos; Chemical communications (Cambridge, England) 57 (2021) 10915–10918; doi:10.1039/d1cc04056a

data_7128978
_publ_section_title
;
 Pd-Catalyzed allylic C-H activation to seven-membered
 <i>N</i>,<i>O</i>-heterocycles.
;
_journal_issue                   83
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10915
_journal_page_last               10918
_journal_paper_doi               10.1039/d1cc04056a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C18 H18 Br N O3 S'
_chemical_formula_sum            'C18 H18 Br N O3 S'
_chemical_formula_weight         408.30
_chemical_name_common            cs1av_2l
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2021-09-09 deposited with the CCDC.	2021-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.174(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3536(8)
_cell_length_b                   9.6592(7)
_cell_length_c                   16.8001(12)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      29.8443
_cell_measurement_theta_min      2.4609
_cell_volume                     1760.3(2)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       'Bruker APEX3 software'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_molecular_graphics    'ORTEP 2014.1 (Farrugia, 2012)'
_computing_publication_material  'IUCr Journals printCIF'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '\k--geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON-III C14'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0866
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            288564
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_min         2.46
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS 3.0'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.469
_exptl_absorpt_correction_T_max  0.746070
_exptl_absorpt_correction_T_min  0.651703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.081
_refine_diff_density_max         2.041
_refine_diff_density_min         -1.332
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         5431
_refine_ls_number_restraints     181
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0615
_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^)+(0.0579P)^2^+4.7000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1499
_refine_ls_wR_factor_ref         0.1572
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4684
_reflns_number_total             5431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04056a2.cif
_cod_data_source_block           21SRA006
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7128978--7128979.cif.
;
_cod_database_code               7128978
_shelx_res_checksum              46391