Two groups of copperII pyridine‒triazole complexes with “open or close” pepper rings and their in vitro antitumor activities
Hong, ZhaoGuo; Zheng, Chu; Luo, Bi; You, Xin; Bian, HeDong; Liang, Hong; Chen, ZhenFeng; Huang, FuPing; RSC Advances 10 (2020) 6297–6305; doi:10.1039/C9RA10677D

data_7239927
_publ_section_title
;
 Two groups of copperII pyridine--triazole complexes with &#x201C;open or
 close&#x201D; pepper rings and their in vitro antitumor activities
;
_journal_issue                   11
_journal_name_full               'RSC Advances'
_journal_page_first              6297
_journal_page_last               6305
_journal_paper_doi               10.1039/C9RA10677D
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C28 H18 Cu2 N10 O10'
_chemical_formula_sum            'C30 H24 Cu2 N10 O11'
_chemical_formula_weight         827.69
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-11-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-26 deposited with the CCDC.	2020-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.081(5)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   11.0710(6)
_cell_length_b                   33.288(2)
_cell_length_c                   26.7627(11)
_cell_measurement_reflns_used    5732
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.3990
_cell_measurement_theta_min      3.7290
_cell_volume                     9710.6(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9784
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -80.00  -6.00   1.00   55.00    --  -18.55 131.00 108.00   74
  2  \w    -92.00  54.00   1.00   55.00    --  -18.55   0.00  60.00  146
  3  \w     -3.00  88.00   1.00   55.00    --   18.86  57.00  30.00   91
  4  \w    -11.00  89.00   1.00   55.00    --   18.86  77.00  60.00  100
  5  \w    -20.00  61.00   1.00   55.00    --   18.86 -99.00 -90.00   81
  6  \w    -95.00 -48.00   1.00   55.00    --  -18.55 178.00 -60.00   47
  7  \w     -7.00  91.00   1.00   55.00    --   18.86  38.00 -60.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0606822000
_diffrn_orient_matrix_UB_12      -0.0063213000
_diffrn_orient_matrix_UB_13      0.0010041000
_diffrn_orient_matrix_UB_21      0.0192636000
_diffrn_orient_matrix_UB_22      -0.0203518000
_diffrn_orient_matrix_UB_23      0.0004614000
_diffrn_orient_matrix_UB_31      0.0133224000
_diffrn_orient_matrix_UB_32      0.0005885000
_diffrn_orient_matrix_UB_33      0.0268935000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1480
_diffrn_reflns_av_unetI/netI     0.1372
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            109498
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.254
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.393
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_description       needle
_exptl_crystal_F_000             5039
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.601
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1339
_refine_ls_number_reflns         17757
_refine_ls_number_restraints     183
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1977
_refine_ls_R_factor_gt           0.1063
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+68.2867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2169
_refine_ls_wR_factor_ref         0.2663
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8449
_reflns_number_total             17757
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra10677d2.cif
_cod_data_source_block           aa_sq
_cod_depositor_comments
'Adding full bibliography for 7239922--7239927.cif.'
_cod_database_code               7239927
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.798
_shelx_estimated_absorpt_t_min   0.649
_reflns_odcompleteness_completeness 99.75
_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 C(H,H) groups
2. Rigid bond restraints
 C84, O24, O23, C82, C81, C83, C78, C78, C80, C65, C66, C68, C69, O20, C56
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
C84 \\sim O24 \\sim O23 \\sim C82 \\sim C81 \\sim C83 \\sim C78 \\sim C78 \\sim
C80 \\sim C65 \\sim C66 \\sim C68 \\sim C69 \\sim O20 \\sim C56: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.005
Uanis(C84) \\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(C82)
\\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C78) \\sim Ueq,
Uanis(C78) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66)
\\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(O20) \\sim Ueq,
Uanis(C56) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
Uanis(C70) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O22) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4.a Riding coordinates:
 C84(H84A,H84B)
4.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C28(H28A,H28B), C42(H42A,H42B), C56(H56A,H56B), C70(H70A,H70B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C13(H13), C15(H15),
 C16(H16), C17(H17), C18(H18), C23(H23), C24(H24), C27(H27), C29(H29), C30(H30),
  C31(H31), C32(H32), C37(H37), C38(H38), C41(H41), C43(H43), C44(H44),
 C45(H45), C46(H46), C51(H51), C52(H52), C55(H55), C57(H57), C58(H58), C59(H59),
  C60(H60), C65(H65), C66(H66), C69(H69), C71(H71), C72(H72), C73(H73),
 C74(H74), C79(H79), C83(H83), C80(H80)
4.d Fitted hexagon refined as free rotating group:
 C79(C78,C83,C82,C81,C80)
;
_shelx_res_checksum              11176
_shelx_fab_checksum              31545
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.258
_oxdiff_exptl_absorpt_empirical_full_min 0.828