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_7710945
_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_formula_moiety
'2(C20 H30 Cl Cu5 N12 O9), C20 H28 Cu5 N12 O8, 4(Cl), 4(H2 O)'
_chemical_formula_sum            'C60 H96 Cl6 Cu15 N36 O30'
_chemical_formula_weight         2967.52
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-29
_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                69.591(6)
_cell_angle_beta                 64.511(7)
_cell_angle_gamma                70.285(6)
_cell_formula_units_Z            1
_cell_length_a                   14.2267(10)
_cell_length_b                   14.4788(10)
_cell_length_c                   16.4283(10)
_cell_measurement_reflns_used    8398
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.2070
_cell_measurement_theta_min      3.8780
_cell_volume                     2791.9(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 0.997
_diffrn_measured_fraction_theta_max 0.834
_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    -15.00  30.00   1.00    2.00    --  -11.20 -99.00-180.00   45
  2  \w    -93.00  72.00   1.00    2.00    --  -11.20   0.00-150.00  165
  3  \w    -68.00 -13.00   1.00    2.50    --  -11.04 -37.00 120.00   55
  4  \w     -6.00  20.00   1.00    2.50    --  -11.04 -77.00 -30.00   26
  5  \w    -13.00  21.00   1.00    2.50    --  -11.04 -99.00  60.00   34
  6  \w    -44.00  -7.00   1.00    2.50    --  -11.04 -19.00 -30.00   37
  7  \w     46.00  73.00   1.00    2.50    --   12.53-178.00  60.00   27
  8  \w     28.00  63.00   1.00    2.50    --   12.53-124.00  14.00   35
;
_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      -0.0402607000
_diffrn_orient_matrix_UB_12      0.0317734000
_diffrn_orient_matrix_UB_13      0.0287026000
_diffrn_orient_matrix_UB_21      0.0079056000
_diffrn_orient_matrix_UB_22      -0.0365583000
_diffrn_orient_matrix_UB_23      0.0398594000
_diffrn_orient_matrix_UB_31      0.0390443000
_diffrn_orient_matrix_UB_32      0.0229537000
_diffrn_orient_matrix_UB_33      -0.0038027000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_unetI/netI     0.0881
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.834
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31010
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.834
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.844
_diffrn_reflns_theta_min         3.277
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.016
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44370
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_description       block
_exptl_crystal_F_000             1485
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.089
_refine_diff_density_min         -1.811
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         13382
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0588P)^2^+2.6444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1481
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9632
_reflns_number_total             13382
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02223k2.cif
_cod_data_source_block           20211229d
_cod_original_cell_volume        2791.8(4)
_cod_database_code               7710945
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1O1Cu1Cl1
_shelx_estimated_absorpt_t_max   0.584
_shelx_estimated_absorpt_t_min   0.584
_diffrn_oxdiff_digest_frames
;
01733e8833e290f32f119312c362d6e19000222b0a5
;
_diffrn_oxdiff_digest_hkl
;
01c8a61861a5a25e3ce46d087c57ef1b32db16
;
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H11B-H10A_$1
 -2.1 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C18A) = Uanis(C18)
4. Others
 Sof(H17C)=Sof(H17D)=Sof(H19C)=Sof(H19D)=Sof(C18A)=Sof(H18C)=Sof(H18D)=1-FVAR(1)
 Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H19A)=Sof(H19B)=FVAR(1)
5.a Free rotating group:
 O10(H10A,H10B), O11(H11A,H11B)
5.b Rotating group:
 O9(H9A,H9B)
5.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C7(H7A,H7B), C8(H8A,H8B), C9(H9C,H9D),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C17(H17A,H17B), C17(H17C,H17D),
  C18(H18A,H18B), C19(H19A,H19B), C19(H19C,H19D), C22(H22A,H22B), C23(H23A,
 H23B), C24(H24A,H24B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B),
 C18A(H18C,H18D)
5.d Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6), N9(H9), N12(H12), N13(H13), N16(H16)
;
_shelx_res_checksum              99641
_shelx_hkl_checksum              42890
_shelx_fab_checksum              71326
_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 1.530
_oxdiff_exptl_absorpt_empirical_full_min 0.606