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_7055623
_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         'C52 H62 Gd2 N10 Ni2 O32'
_chemical_formula_sum            'C52 H62 Gd2 N10 Ni2 O32'
_chemical_formula_weight         1771.03
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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                 97.274(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.1274(7)
_cell_length_b                   12.9696(7)
_cell_length_c                   17.1643(8)
_cell_measurement_reflns_used    5259
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      69.6000
_cell_measurement_theta_min      10.3730
_cell_volume                     3340.5(3)
_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
;
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 0.985
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details
;
  1 omega   98.00  123.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000    0.0000 17

  2 omega   93.00  133.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000  120.0000 27

  3 omega  148.00  175.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000  120.0000 18

  4 omega  119.00  146.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000    0.0000 18

  5 omega   60.00   87.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000    0.0000 18

  6 omega   44.00  123.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   30.0000 53

  7 omega   43.00   94.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000    0.0000 34

  8 omega   36.00   94.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -60.0000 39

  9 omega   44.00  131.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -63.0000   30.0000 58

 10 omega   43.00  112.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -150.0000 46

 11 omega   35.00   93.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000    0.0000 39

 12 omega   36.00   72.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   90.0000 24

 13 omega   41.00   68.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  120.0000 18

 14 omega   43.00   89.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   60.0000 31

 15 omega   43.00  107.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   30.0000 43

 16 omega    5.00   86.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000  -90.0000 54

 17 omega  -14.00   23.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000 -180.0000 25
;
_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      0.0872110000
_diffrn_orient_matrix_UB_12      -0.0110367000
_diffrn_orient_matrix_UB_13      0.0564121000
_diffrn_orient_matrix_UB_21      -0.0121971000
_diffrn_orient_matrix_UB_22      -0.1178318000
_diffrn_orient_matrix_UB_23      0.0000476000
_diffrn_orient_matrix_UB_31      0.0528806000
_diffrn_orient_matrix_UB_32      -0.0089172000
_diffrn_orient_matrix_UB_33      -0.0707801000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12619
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.891
_diffrn_reflns_theta_min         10.399
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.111
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52678
_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.
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    1.761
_exptl_crystal_description       block
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.068
_refine_diff_density_min         -1.408
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6098
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0661P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1152
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5111
_reflns_number_total             6098
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj00855k1.cif
_cod_data_source_block           d743
_cod_depositor_comments
'Adding full bibliography for 7055617--7055625.cif.'
_cod_database_code               7055623
_reflns_odcompleteness_completeness 98.45
_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.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:
 C5AA(H5AA,H5AB,H5AC), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C26(H26A,H26B,H26C)
;
_olex2_date_sample_data_collection 2015-08-28
_olex2_submission_special_instructions 'No special instructions were received'