Multicomponent Pyrazole Synthesis from Alkynes, Nitriles, and Ti Imidos via Oxidatively Induced N-N Bond Coupling.
Pearce, Adam J.; Harkins, Robin P.; Reiner, Benjamin R.; Wotal, Alexander C.; Dunscomb, Rachel J.; Tonks, Ian A.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b13173

data_4134215
_publ_section_title
;
 Multicomponent Pyrazole Synthesis from Alkynes, Nitriles, and Ti Imidos
 via Oxidatively Induced N-N Bond Coupling.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b13173
_journal_year                    2020
_chemical_formula_moiety         'C33 H30 Cl2 N4 Ti'
_chemical_formula_sum            'C33 H30 Cl2 N4 Ti'
_chemical_formula_weight         601.41
_space_group_crystal_system      triclinic
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_cell_length_c                   14.3737(5)
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    100(2)
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_cell_measurement_theta_min      2.345
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_computing_cell_refinement       'SAINT, Bruker'
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_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'Shelxle-(Rev. 825) (Huebschle, C. B., 2011)'
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_diffrn_ambient_temperature      100(2)
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_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  '\f and \w scans'
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_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_h_max       12
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_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34274
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
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_diffrn_reflns_theta_max         29.668
_diffrn_reflns_theta_min         2.302
_diffrn_source                   'Bruker Photon-III CMOS'
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.7061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       Block
_exptl_crystal_F_000             624
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_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         8254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0357P)^2^+1.0246P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0954
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6950
_reflns_number_total             8254
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            19093.cif
_cod_data_source_block           19093
_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/ACS/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 
;
_cod_database_code               4134215
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.949
_shelx_estimated_absorpt_t_max   0.995
_shelx_res_checksum              42441
_shelx_hkl_checksum              44048