Iodine-Catalyzed Diazenylation with Arylhydrazine Hydrochlorides in Air.
Barak, Dinesh S.; Dighe, Shashikant U.; Avasthi, Ilesha; Batra, Sanjay; The Journal of organic chemistry 83 (2018) 3537–3546; doi:10.1021/acs.joc.7b03149

data_4035508
_publ_section_title
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 Iodine-Catalyzed Diazenylation with Arylhydrazine Hydrochlorides in Air.
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_journal_issue                   7
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              3537
_journal_page_last               3546
_journal_paper_doi               10.1021/acs.joc.7b03149
_journal_volume                  83
_journal_year                    2018
_chemical_formula_sum            'C16 H13 N3 O'
_chemical_formula_weight         263.29
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                90.000
_cell_formula_units_Z            16
_cell_length_a                   15.832(4)
_cell_length_b                   17.439(5)
_cell_length_c                   19.676(6)
_cell_measurement_reflns_used    4784
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      4.1
_cell_volume                     5432(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Advance diffractometer'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35782
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         4.10
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.9851
_exptl_absorpt_correction_T_min  0.9819
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle-like
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         4784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+3.9718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1096
_reflns_number_gt                4055
_reflns_number_total             4784
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo7b03149_si_002.cif
_cod_data_source_block           3ai
_cod_depositor_comments
;

2020-04-07
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
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_cod_original_formula_sum        'C32 H26 N6 O2'
_cod_original_formula_units_Z    8
_cod_original_formula_weight     526.59
_cod_database_code               4035508