An easy synthetic access to new pyrazole spiro derivatives from 3-amino-1-phenyl-2-pyrazolin-5-one
Zaiter, Jamila; Achibat, Hanane; Amiri, Ouafa; Hafid, Abderrafia; Khouili, Mostafa; Rakib, El Mostapha; Neves, Cláudia M. B.; Neves, Maria Graça P. M. S.; Silva, Artur M. S.; Cavaleiro, José A. S.; Almeida Paz, Filipe A.; Faustino, Maria Amparo F.; New J. Chem. 39 (2015) 6738–; doi:10.1039/C5NJ01306B

data_7055001
_publ_section_title
;
 An easy synthetic access to new pyrazole spiro derivatives from
 3-amino-1-phenyl-2-pyrazolin-5-one
;
_journal_issue                   9
_journal_name_full               'New J. Chem.'
_journal_page_first              6738
_journal_paper_doi               10.1039/C5NJ01306B
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety
'2(C32 H26 N6 O2), 3.5(C H Cl3), 0.5(C3 H6 O)'
_chemical_formula_sum            'C69 H58.5 Cl10.5 N12 O4.5'
_chemical_formula_weight         1500.00
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             '7 July 2015'
_audit_creation_method           'SHELXL-2014/6, manual editing plus enCIFer'
_audit_update_record
;
2015-07-07 deposited with the CCDC.
2015-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                78.971(4)
_cell_angle_beta                 85.227(5)
_cell_angle_gamma                81.247(4)
_cell_formula_units_Z            2
_cell_length_a                   11.4963(12)
_cell_length_b                   16.0196(17)
_cell_length_c                   20.763(2)
_cell_measurement_reflns_used    9823
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.26
_cell_measurement_theta_min      2.36
_cell_volume                     3703.7(7)
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_data_collection       'APEX2 2012.4 (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 QUEST '
_diffrn_measurement_method       '\w / \f scans'
_diffrn_radiation_monochromator  'Multi-layer X-ray mirror'
_diffrn_radiation_source         'Sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            78963
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         3.572
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.450
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS V2012/1 (Bruker AXS Inc.) 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1542
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.020
_exptl_transmission_factor_max   0.7458
_exptl_transmission_factor_min   0.6836
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1128
_refine_ls_number_reflns         13499
_refine_ls_number_restraints     998
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1132
_refine_ls_R_factor_gt           0.0812
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1127P)^2^+5.2229P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2063
_refine_ls_wR_factor_ref         0.2254
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9582
_reflns_number_total             13499
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj01306b2.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_space_group_crystal_system' value 'Triclinic' changed to
'triclinic' according to
/usr/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.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/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 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7055001.cif.
;
_cod_original_formula_sum        'C69 H58.50 Cl10.50 N12 O4.50'
_cod_database_code               7055001
_shelx_estimated_absorpt_t_min   0.948
_shelx_estimated_absorpt_t_max   0.991
_shelxl_version_number           2014/6
_shelx_res_checksum              50001