Reactivity of di(amidoxime) ligand in the presence of Cu(II)/Ni(II)
Liu, Tingting; Liu, Qian; Xue, Yun; Yang, Suliang; Ma, Fuqiu; Tian, Guoxin; Dalton Transactions  (2022) –; doi:10.1039/D2DT02223K

data_7710944
_publ_section_title
;
 Reactivity of di(amidoxime) ligand in the presence of Cu(II)/Ni(II)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02223K
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C15 H24 Cl2 Cu3 N9 O3, Cl'
_chemical_formula_sum            'C15 H24 Cl3 Cu3 N9 O3'
_chemical_formula_weight         675.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-03-05 deposited with the CCDC.	2022-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.7421(7)
_cell_length_b                   26.2769(12)
_cell_length_c                   15.0315(7)
_cell_measurement_reflns_used    3653
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.5820
_cell_measurement_theta_min      4.2860
_cell_volume                     5427.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.864
_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    -61.00  34.00   1.00   10.00    --   12.61 -57.00 -90.00   95
  2  \w    -65.00 -10.00   1.00   10.00    --   12.61 -19.00 150.00   55
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0051186000
_diffrn_orient_matrix_UB_12      -0.0059402000
_diffrn_orient_matrix_UB_13      0.0458163000
_diffrn_orient_matrix_UB_21      -0.0481993000
_diffrn_orient_matrix_UB_22      0.0083928000
_diffrn_orient_matrix_UB_23      0.0077993000
_diffrn_orient_matrix_UB_31      -0.0174636000
_diffrn_orient_matrix_UB_32      -0.0249843000
_diffrn_orient_matrix_UB_33      -0.0084126000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.864
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5216
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.865
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.810
_diffrn_reflns_theta_min         4.018
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.658
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_description       block
_exptl_crystal_F_000             2712
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.321
_refine_diff_density_min         -1.317
_refine_diff_density_rms         0.143
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.05(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         2729
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0570P)^2^+102.0854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1287
_refine_ls_wR_factor_ref         0.1314
_reflns_Friedel_coverage         0.935
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.867
_reflns_number_gt                2597
_reflns_number_total             2729
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02223k2.cif
_cod_data_source_block           20211103f
_cod_database_code               7710944
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1O1Cu1
_shelx_estimated_absorpt_t_max   0.691
_shelx_estimated_absorpt_t_min   0.556
_diffrn_oxdiff_digest_frames
;
011782be560ef170b19b5af0b7e4615fcc00158e293
;
_diffrn_oxdiff_digest_hkl
;
0169860f7aec052e9a012980fdc4b23da0241b
;
_reflns_odcompleteness_completeness 99.42
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.95(4)
 0.05(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C8) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Cl2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C2) \\sim Ueq: with sigma of 0.0056 and sigma for terminal atoms of 0.0112
Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: Cl2(0.5) H8A(0.5) H8B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C7(H7A,H7B), C8(H8A,H8B)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), N5(H5)
;
_shelx_res_checksum              23435
_shelx_hkl_checksum              14433
_shelx_fab_checksum              45800
_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 1.261
_oxdiff_exptl_absorpt_empirical_full_min 0.760