Comparative studies on conventional and solvent-free synthesis toward hydrazones: application of PXRD and chemometric data analysis in mechanochemical reaction monitoring
Pisk, Jana; Hrenar, Tomica; Rubčić, Mirta; Pavlović, Gordana; Damjanović, Vladimir; Lovrić, Jasna; Cindrić, Marina; Vrdoljak, Višnja; CrystEngComm 20 (2018) 1804–; doi:10.1039/C7CE02136D

data_7230142
_publ_section_title
;
 Comparative studies on conventional and solvent-free synthesis toward
 hydrazones: application of PXRD and chemometric data analysis in
 mechanochemical reaction monitoring
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              1804
_journal_paper_doi               10.1039/C7CE02136D
_journal_volume                  20
_journal_year                    2018
_chemical_formula_sum            'C15 H17 N3 O4'
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_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
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_atom_sites_solution_hydrogens   mixed
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;
2017-11-29 deposited with the CCDC.
2018-02-12 downloaded from the CCDC.
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_cell_angle_gamma                90
_cell_formula_units_Z            4
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'MERCURY 3.8. (CCDC, 2016)'
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_diffrn_ambient_temperature      296(2)
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_diffrn_reflns_limit_k_min       -16
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.499
_diffrn_reflns_theta_min         4.511
_diffrn_source                   'Enhance (Mo) X-ray Source'
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35.
Empirical absorption correction 
using spherical harmonics,
 implemented in SCALE3 ABSPACK 
scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       plate
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.177
_refine_diff_density_min         -0.191
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_refine_ls_abs_structure_details
;
 Flack x determined using 332 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.4(10)
_refine_ls_extinction_method     none
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_refine_ls_number_parameters     218
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_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.2087
_refine_ls_R_factor_gt           0.0769
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.1091
_reflns_Friedel_coverage         0.751
_reflns_Friedel_fraction_full    0.942
_reflns_Friedel_fraction_max     0.947
_reflns_number_gt                1467
_reflns_number_total             3564
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce02136d2.cif
_cod_data_source_block           4bH2Oexp3070
_cod_depositor_comments
'Adding full bibliography for 7230137--7230144.cif.'
_cod_database_code               7230142
_shelx_shelxl_version_number     2014/7
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