Heptafluoroisopropyl diazomethane (i-C3F7CHN2): in situ generation and synthesis of pyrazoles
Mykhailiuk, Pavel K.; Org. Biomol. Chem.  (2017) –; doi:10.1039/C7OB01579H

data_7155767
_publ_section_title
;
 Heptafluoroisopropyl diazomethane (i-C3F7CHN2): in situ generation and
 synthesis of pyrazoles
;
_journal_name_full               'Org. Biomol. Chem.'
_journal_paper_doi               10.1039/C7OB01579H
_journal_year                    2017
_chemical_formula_sum            'C11 H9 F7 N2 O'
_chemical_formula_weight         318.20
_space_group_IT_number           2
_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
;
2017-06-23 deposited with the CCDC.
2017-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                68.673(13)
_cell_angle_beta                 90.021(8)
_cell_angle_gamma                89.803(11)
_cell_formula_units_Z            12
_cell_length_a                   12.6081(12)
_cell_length_b                   16.880(3)
_cell_length_c                   19.0740(16)
_cell_measurement_temperature    100(2)
_cell_volume                     3781.4(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1629
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24142
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.179
_exptl_absorpt_correction_T_max  0.9946
_exptl_absorpt_correction_T_min  0.9651
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1136
_refine_ls_number_reflns         24236
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.2050
_refine_ls_R_factor_gt           0.1201
_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^)+(0.1320P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2760
_refine_ls_wR_factor_ref         0.3391
_reflns_number_gt                11489
_reflns_number_total             24236
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ob01579h2.cif
_cod_data_source_block           tolm329
_cod_original_cell_volume        3781.3(8)
_cod_database_code               7155767