Direct synthesis of enone-hydrazones under solvent free and additive free conditions.
He, Kun; Zeng, Weikun; Yu, Xianglin; Zhou, Jun; Jin, Yi; Organic & biomolecular chemistry 23 (2025) 377–382; doi:10.1039/d4ob01578a

data_7160208
_publ_section_title
;
 Direct synthesis of enone-hydrazones under solvent free and additive free
 conditions.
;
_journal_issue                   2
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              377
_journal_page_last               382
_journal_paper_doi               10.1039/d4ob01578a
_journal_volume                  23
_journal_year                    2025
_chemical_formula_moiety         'C24 H22 N2 O'
_chemical_formula_sum            'C24 H22 N2 O'
_chemical_formula_weight         354.43
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_atom_sites_solution_hydrogens   mixed
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;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
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_audit_update_record
;
2022-07-15 deposited with the CCDC.	2024-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.555(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.550(19)
_cell_length_b                   6.415(9)
_cell_length_c                   21.40(3)
_cell_measurement_reflns_used    602
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      16.89
_cell_measurement_theta_min      2.85
_cell_volume                     1964(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1497
_diffrn_reflns_av_unetI/netI     0.1862
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       7
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_diffrn_reflns_limit_l_max       25
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_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_min         1.862
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
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_exptl_crystal_description       block
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'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^] where P=(Fo^2^+2Fc^2^)/3'
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_reflns_number_gt                1281
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_reflns_threshold_expression     'I > 2\s(I)'
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'Adding full bibliography for 7160207--7160208.cif.'
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_shelx_estimated_absorpt_t_max   0.996
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_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.099) H2(0.116) H3(0.12) H4(0.116) H5(0.099) H8(0.085)
 H9(0.089) H12(0.079) H13(0.092) H14(0.098) H15(0.094) H16(0.082) H18(0.085)
 H21(0.093) H22(0.083) H23A(0.163) H23B(0.163) H23C(0.163) H24A(0.145)
 H24B(0.145) H24C(0.145)
 Fixed X: H1(0.325949) H2(0.270416) H3(0.112509) H4(0.010048) H5(0.063167)
 H8(0.364449) H9(0.422017) H12(0.236005) H13(0.086306) H14(-0.028659)
 H15(0.004742) H16(0.153207) H18(0.285716) H21(0.506962) H22(0.439166)
 H23A(0.398334) H23B(0.313861) H23C(0.301664) H24A(0.530786) H24B(0.437295)
 H24C(0.513453)
 Fixed Y: H1(1.208115) H2(1.489413) H3(1.537809) H4(1.309826) H5(1.035367)
 H8(0.893183) H9(0.628082) H12(0.649167) H13(0.720954) H14(0.470461)
 H15(0.150887) H16(0.072852) H18(0.127131) H21(-0.239326) H22(0.047012) H23A(-
 0.192765) H23B(-0.316497) H23C(-0.081984) H24A(-0.476618) H24B(-0.529431)
 H24C(-0.392423)
 Fixed Z: H1(-0.147684) H2(-0.211414) H3(-0.24337) H4(-0.211583) H5(-0.144936)
 H8(-0.11942) H9(-0.056043) H12(0.092148) H13(0.108394) H14(0.086353)
 H15(0.048056) H16(0.03347) H18(0.161349) H21(0.080396) H22(0.026838)
 H23A(0.273363) H23B(0.23451) H23C(0.251912) H24A(0.163753) H24B(0.186906)
 H24C(0.229382)
;
_shelx_res_checksum              33580
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'