Thermal Rearrangements of 3- and 4-Pyrazoles Prepared by Reactions of 9-Diazofluoren with Methyl Tetrolate and Methyl 3-Phenylpropiolate
Vasin, V..; Popkova, Yu..; Bezrukova, Ye.V.; Razin, V.V.; Somov, N.V.; Russian Journal of Organic Chemistry 54 (2018) 1189–1199; doi:10.1134/S1070428018080122

data_4038961
_publ_section_title
;
 Thermal Rearrangements of 3- and 4-Pyrazoles Prepared by Reactions of
 9-Diazofluoren with Methyl Tetrolate and Methyl 3-Phenylpropiolate
;
_journal_issue                   8
_journal_name_full
;
 Russian Journal of Organic Chemistry
;
_journal_page_first              1189
_journal_page_last               1199
_journal_paper_doi               10.1134/S1070428018080122
_journal_volume                  54
_journal_year                    2018
_chemical_formula_sum            'C22 H16 N2 O2 S'
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_space_group_name_Hall           '-P 2ybc'
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_symmetry_space_group_name_Hall  '-P 2ybc'
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
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        CrysAlisPro, Agilent Technologies,
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        CrysAlisPro, Agilent Technologies,
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        (compiled Jan 23 2012,18:06:46)
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_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 16.0302
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_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0086197
_diffrn_orient_matrix_UB_12      -0.0305823
_diffrn_orient_matrix_UB_13      0.0321778
_diffrn_orient_matrix_UB_21      -0.0524671
_diffrn_orient_matrix_UB_22      -0.0124266
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_diffrn_orient_matrix_UB_31      0.0576632
_diffrn_orient_matrix_UB_32      -0.006737
_diffrn_orient_matrix_UB_33      -0.0360145
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
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_diffrn_reflns_limit_l_max       13
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_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
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_diffrn_reflns_theta_max         30.504
_diffrn_reflns_theta_min         3.615
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.95876
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        CrysAlisPro, Agilent Technologies,
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        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       prism
_exptl_crystal_F_000             776
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_exptl_crystal_size_mid          0.4518
_exptl_crystal_size_min          0.3791
_refine_diff_density_max         0.363
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_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
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_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.7524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1367
_reflns_Friedel_coverage         0
_reflns_number_gt                4852
_reflns_number_total             5500
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tmp7y2w_8qe
_cod_data_source_block           m_207_p_060912
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4038961