Synthesis and biological evaluation of heterocyclic hydrazone transition metal complexes as potential anticancer agents
jungang, deng; Yunpeng, Du; Wei, Chen; Xiang, Fu; Hang, Deng; RSC Adv.  (2016) –; doi:10.1039/C6RA23477A

data_7227095
_publ_section_title
;
 Synthesis and biological evaluation of heterocyclic hydrazone transition
 metal complexes as potential anticancer agents
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA23477A
_journal_year                    2016
_chemical_formula_moiety         'Cl, C17 H14 N3 O2, H2 O'
_chemical_formula_sum            'C17 H16 Cl N3 O3'
_chemical_formula_weight         345.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-05-14
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-08-23 deposited with the CCDC.
2016-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.578(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.2591(3)
_cell_length_b                   18.7570(10)
_cell_length_c                   12.2090(5)
_cell_measurement_reflns_used    2199
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.5247
_cell_measurement_theta_min      2.8809
_cell_volume                     1615.90(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 15.9784
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -14.00   16.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2889  -99.0000   30.0000 30

  2 omega  -48.00   40.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3827  -57.0000 -120.0000 88

  3 omega   23.00   49.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3827   57.0000  120.0000 26

  4 omega   -3.00   88.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3827  -19.0000  -90.0000 91

  5 omega  -45.00    5.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3827   19.0000   30.0000 50
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0059405000
_diffrn_orient_matrix_UB_12      -0.0355549000
_diffrn_orient_matrix_UB_13      -0.0202195000
_diffrn_orient_matrix_UB_21      -0.0900879000
_diffrn_orient_matrix_UB_22      0.0074886000
_diffrn_orient_matrix_UB_23      -0.0356661000
_diffrn_orient_matrix_UB_31      0.0442309000
_diffrn_orient_matrix_UB_32      0.0103973000
_diffrn_orient_matrix_UB_33      -0.0435143000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7902
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         2.89
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.257
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'yellowish yellow'
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.174
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.1135
_reflns_number_gt                2083
_reflns_number_total             3289
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra23477a1.cif
_cod_data_source_block           1124-yf-jm-n13-2-01
_cod_database_code               7227095
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C11(H11), C4(H4), C8(H8), C10(H10), C5(H5), C13(H13), C2(H2B),
  C14(H14), C16(H16), C1(H1A), C15(H15)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2A)
;
_olex2_submission_special_instructions 'No special instructions were received'