Rearrangements of 3H-PyrazolesAdducts of Dimethyl Acetylenedicarboxylate with Diphenyldiazomethane and 9-Diazofluorene
Vasin, V.A.; Razin, V.V.; Bezrukova, E.V.; Popkova, Yu.A.; Somov, N.V.; Russian Journal of Organic Chemistry 54 (2018) 892–900; doi:10.1134/S1070428018060118

data_4038960
_publ_section_title
;
 Rearrangements of 3H-PyrazolesAdducts of Dimethyl Acetylenedicarboxylate
 with Diphenyldiazomethane and 9-Diazofluorene
;
_journal_issue                   6
_journal_name_full
;
 Russian Journal of Organic Chemistry
;
_journal_page_first              892
_journal_page_last               900
_journal_paper_doi               10.1134/S1070428018060118
_journal_volume                  54
_journal_year                    2018
_chemical_formula_sum            'C19 H14 N2 O4'
_chemical_formula_weight         334.32
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-01-17T11:30:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 132.96(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   7.2325(5)
_cell_length_c                   23.507(4)
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_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.739
_cell_measurement_theta_min      3.573
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_computing_data_collection       'CrysAlisPro 1.171.39.8e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.8e (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.004599
_diffrn_orient_matrix_UB_12      0.0074123
_diffrn_orient_matrix_UB_13      0.0317131
_diffrn_orient_matrix_UB_21      0.0591725
_diffrn_orient_matrix_UB_22      0.0615292
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_diffrn_orient_matrix_UB_32      0.0760516
_diffrn_orient_matrix_UB_33      -0.0183739
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0769
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
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_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         3.575
_diffrn_source                   'fine-focus sealed X-ray tube'
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_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.45141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.39.8e (Rigaku Oxford Diffraction, 2015)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       prism
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.514
_exptl_crystal_size_mid          0.334
_exptl_crystal_size_min          0.152
_refine_diff_density_max         0.22
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.032
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3908
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+0.3516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1206
_reflns_Friedel_coverage         0
_reflns_number_gt                2960
_reflns_number_total             3908
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tmpngqeiemg
_cod_data_source_block           my-190
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4038960