Generation of (2-oxoindolin-3-yl)methanesulfonohydrazides via a photo-induced reaction of N-(2-iodoaryl)acrylamide, DABSO, and hydrazine
Zhou, Kaida; Xia, Hongguang; Wu, Jie; Organic Chemistry Frontiers 3 (2016) 865–; doi:10.1039/C6QO00163G

data_1553463
_publ_section_title
;
 Generation of (2-oxoindolin-3-yl)methanesulfonohydrazides via a
 photo-induced reaction of N-(2-iodoaryl)acrylamide, DABSO, and hydrazine
;
_journal_issue                   7
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              865
_journal_paper_doi               10.1039/C6QO00163G
_journal_volume                  3
_journal_year                    2016
_chemical_formula_sum            'C17 H25 Cl2 N3 O4 S'
_chemical_formula_weight         438.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-12-17 deposited with the CCDC.
2016-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                74.634(5)
_cell_angle_beta                 62.808(5)
_cell_angle_gamma                65.132(5)
_cell_formula_units_Z            2
_cell_length_a                   10.820(6)
_cell_length_b                   10.975(6)
_cell_length_c                   11.163(6)
_cell_measurement_reflns_used    2942
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.82
_cell_measurement_theta_min      2.38
_cell_volume                     1065.4(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5239
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         2.054
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
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_exptl_crystal_description       block
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_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       0.028(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         3666
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0806
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.1584P)^2^+0.8442P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2404
_refine_ls_wR_factor_ref         0.2518
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2999
_reflns_number_total             3666
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6qo00163g2.cif
_cod_data_source_block           a51020a
_cod_original_cell_volume        1065.4(9)
_cod_database_code               1553463
_shelx_estimated_absorpt_t_min   0.725
_shelx_estimated_absorpt_t_max   0.814
_shelxl_version_number           2013-2
_shelx_res_checksum              97031
_shelx_hkl_checksum              90714