Nine self-assembled nickel(ii)‒lanthanide(iii) heterometallic complexes constructed from a Salamo-type bisoxime and bearing a N- or O-donor auxiliary ligand: syntheses, structures and magnetic properties
Dong, Wen-Kui; Ma, Jian-Chun; Zhu, Li-Chun; Zhang, Yang; New J. Chem. 40 (2016) 6998–; doi:10.1039/C6NJ00855K

data_7055620
_publ_section_title
;
 Nine self-assembled nickel(ii)--lanthanide(iii) heterometallic complexes
 constructed from a Salamo-type bisoxime and bearing a N- or O-donor
 auxiliary ligand: syntheses, structures and magnetic properties
;
_journal_issue                   8
_journal_name_full               'New J. Chem.'
_journal_page_first              6998
_journal_paper_doi               10.1039/C6NJ00855K
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C28 H26 N7 Ni O15 Tb'
_chemical_formula_sum            'C28 H26 N7 Ni O15 Tb'
_chemical_formula_weight         918.19
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2015-09-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-11-01 deposited with the CCDC.
2016-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.096(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2398(4)
_cell_length_b                   20.6747(7)
_cell_length_c                   15.2449(5)
_cell_measurement_reflns_used    6068
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      69.6550
_cell_measurement_theta_min      4.2730
_cell_volume                     3225.3(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
  1 omega  146.00  176.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000   30.0000 20

  2 omega   99.00  178.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -60.0000 53

  3 omega   92.00  119.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000  -90.0000 18

  4 omega   86.00  140.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000 -120.0000 36

  5 omega   54.00   94.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -30.0000 27

  6 omega   63.00  130.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -91.0000  -60.0000 45

  7 omega   87.00  114.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -120.0000 18

  8 omega   51.00   78.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -120.0000 18

  9 omega   45.00   99.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  -90.0000 36

 10 omega   48.00  103.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  -30.0000 37

 11 omega   44.00   92.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000 -150.0000 32

 12 omega   39.00   69.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -90.0000 20

 13 omega   42.00  123.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -150.0000 54

 14 omega   38.00   95.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   38.0000   30.0000 38

 15 omega   55.00  113.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   38.0000  150.0000 39

 16 omega   36.00   91.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  120.0000 37

 17 omega   39.00   67.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -91.0000  120.0000 19

 18 omega   46.00  109.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  120.0000 42

 19 omega   36.00   79.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000   60.0000 29

 20 omega   36.00   84.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   30.0000 32

 21 omega   28.00  101.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -132.0000 -135.0000 49

 22 omega   -1.00   72.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000 -120.0000 49

 23 omega   -6.00   19.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   30.0000 17

 24 omega  -15.00   55.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000   60.0000 47

 25 omega  -13.00   15.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 19

 26 omega   27.00   66.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 26

 27 omega  -62.00  -36.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  132.0000  -65.0000 17

 28 omega  -65.00  -38.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   30.0000 18
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0511612000
_diffrn_orient_matrix_UB_12      -0.0697108000
_diffrn_orient_matrix_UB_13      0.0113628000
_diffrn_orient_matrix_UB_21      0.0139141000
_diffrn_orient_matrix_UB_22      0.0103503000
_diffrn_orient_matrix_UB_23      0.0999434000
_diffrn_orient_matrix_UB_31      -0.1408765000
_diffrn_orient_matrix_UB_32      -0.0243040000
_diffrn_orient_matrix_UB_33      0.0100570000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8791
_diffrn_reflns_point_group_measured_fraction_full 0.695
_diffrn_reflns_point_group_measured_fraction_max 0.681
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.716
_diffrn_reflns_theta_min         4.277
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.125
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.891
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.006(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         4154
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0697P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1038
_reflns_Friedel_coverage         0.394
_reflns_Friedel_fraction_full    0.402
_reflns_Friedel_fraction_max     0.386
_reflns_number_gt                4065
_reflns_number_total             4154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj00855k1.cif
_cod_data_source_block           d777
_cod_depositor_comments
'Adding full bibliography for 7055617--7055625.cif.'
_cod_original_cell_volume        3225.24(19)
_cod_database_code               7055620
_reflns_odcompleteness_completeness 98.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O15) \\sim Ueq, Uanis(O15') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Fixed Sof: O15'(0.5) O15(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C15(H15), C16(H16), C17(H17),
 C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27), C28(H28)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C)
;
_olex2_date_sample_data_collection 2015-08-31
_olex2_submission_special_instructions 'No special instructions were received'