Iodine-mediated cross-dehydrogenative coupling of pyrazolones and alkenes.
Yang, Kai; Bao, Xiaoze; Yao, Ye; Qu, Jingping; Wang, Baomin; Organic & biomolecular chemistry 16 (2018) 6275–6283; doi:10.1039/c8ob01645c

data_7156368
_publ_section_title
;
 Iodine-mediated cross-dehydrogenative coupling of pyrazolones and
 alkenes.
;
_journal_issue                   34
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              6275
_journal_page_last               6283
_journal_paper_doi               10.1039/c8ob01645c
_journal_volume                  16
_journal_year                    2018
_chemical_formula_sum            'C30 H22 N2 O'
_chemical_formula_weight         426.50
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_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-09-05 deposited with the CCDC.
2018-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                72.018(3)
_cell_angle_beta                 70.400(4)
_cell_angle_gamma                89.928(4)
_cell_formula_units_Z            2
_cell_length_a                   9.6135(5)
_cell_length_b                   10.5171(5)
_cell_length_c                   12.3679(5)
_cell_measurement_reflns_used    1954
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.383
_cell_measurement_theta_min      2.3655
_cell_volume                     1113.15(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_av_sigmaI/netI    0.0435
_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       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9950
_diffrn_reflns_theta_full        26.80
_diffrn_reflns_theta_max         26.80
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.077
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             448
_refine_diff_density_max         0.134
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4745
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0749P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1518
_reflns_number_gt                2875
_reflns_number_total             4745
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8ob01645c2.cif
_cod_data_source_block           0
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

 Adding full bibliography for 7156368.cif.
;
_cod_original_cell_volume        1113.15(9)
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               7156368