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_7055624
_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         'C50 H54 N10 Ni2 O30 Tb2'
_chemical_formula_sum            'C50 H54 N10 Ni2 O30 Tb2'
_chemical_formula_weight         1710.29
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-26
_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                99.027(6)
_cell_angle_beta                 95.068(5)
_cell_angle_gamma                101.985(7)
_cell_formula_units_Z            1
_cell_length_a                   10.5724(8)
_cell_length_b                   12.5483(12)
_cell_length_c                   13.8671(7)
_cell_measurement_reflns_used    3843
_cell_measurement_temperature    296.71(10)
_cell_measurement_theta_max      25.3830
_cell_measurement_theta_min      3.5040
_cell_volume                     1763.3(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
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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_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_environment      air
_diffrn_ambient_temperature      296.71(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -46.00   41.00   1.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -57.0000   30.0000 58

  2 omega  -19.00   11.00   1.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1479  -99.0000  -30.0000 20

  3 omega  -14.00   25.00   1.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1479  -99.0000   60.0000 26

  4 omega  -36.00   36.00   1.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -57.0000  150.0000 48

  5 omega  -50.00   40.00   1.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -38.0000  -90.0000 60

  6 omega  -20.00   55.00   1.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -99.0000  -90.0000 50
;
_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      0.0260956000
_diffrn_orient_matrix_UB_12      -0.0472838000
_diffrn_orient_matrix_UB_13      -0.0127515000
_diffrn_orient_matrix_UB_21      -0.0604205000
_diffrn_orient_matrix_UB_22      -0.0347874000
_diffrn_orient_matrix_UB_23      0.0046572000
_diffrn_orient_matrix_UB_31      -0.0211450000
_diffrn_orient_matrix_UB_32      -0.0021945000
_diffrn_orient_matrix_UB_33      -0.0504059000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0811
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13785
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_min         3.493
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.593
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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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    1.611
_exptl_crystal_description       block
_exptl_crystal_F_000             850
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.226
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         6907
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0268P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
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_reflns_number_gt                5551
_reflns_number_total             6907
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj00855k1.cif
_cod_data_source_block           d791
_cod_depositor_comments
'Adding full bibliography for 7055617--7055625.cif.'
_cod_database_code               7055624
_reflns_odcompleteness_completeness 99.72
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C11(H11), C15(H15), C16(H16), C17(H17),
 C19(H19), C24(H24), C25(H25)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_olex2_date_sample_data_collection 2015-07-03
_olex2_submission_special_instructions 'No special instructions were received'