Three series of heterometallic Ni <sup>II</sup> –Ln <sup>III</sup> Schiff base complexes: synthesis, crystal structures and magnetic characterization
Jiang, Lin; Liu, Yue; Liu, Xin; Tian, Jinlei; Yan, Shiping; Dalton Transactions 46 (2017) 12558–12573; doi:10.1039/C7DT02351K

data_1546873
_publ_section_title
;
 Three series of heterometallic Ni <sup>II</sup> --Ln <sup>III</sup>
 Schiff base complexes: synthesis, crystal structures and magnetic
 characterization
;
_journal_issue                   37
_journal_name_full               'Dalton Transactions'
_journal_page_first              12558
_journal_page_last               12573
_journal_paper_doi               10.1039/C7DT02351K
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C31 H24 F15 Gd N2 Ni O12'
_chemical_formula_sum            'C31 H24 F15 Gd N2 Ni O12'
_chemical_formula_weight         1117.48
_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_block_doi                 10.5517/ccdc.csd.cc1p7lbv
_audit_creation_date             2017-07-31
_audit_creation_method
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  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_audit_update_record
;
2017-08-14 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.715(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.293(4)
_cell_length_b                   12.677(2)
_cell_length_c                   16.658(3)
_cell_measurement_reflns_used    11940
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
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_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
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_computing_data_collection
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CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
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_computing_data_reduction
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CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
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_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      113
_diffrn_detector                 PILT
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_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -105.0000 - 75.0000
         Image width: 0.5000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 45.0435
              2theta: -15.1203
scan:
    Number of images: 300
               Slice: -105.0000 - 45.0000
         Image width: 0.5000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 45.0435
              2theta: -15.1203
scan:
    Number of images: 200
               Slice: -105.0000 - -5.0000
         Image width: 0.5000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 45.0435
              2theta: -15.1203
;
_diffrn_measurement_device
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AFC10: Fixed Chi 2 circle
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_diffrn_measurement_device_type
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Rigaku Pilatus 200K
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_diffrn_orient_matrix_UB_31      0.029387
_diffrn_orient_matrix_UB_32      0.036473
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_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       21
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_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32172
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         3.032
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.345
_exptl_absorpt_correction_T_max  0.626
_exptl_absorpt_correction_T_min  0.603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear grayish gray'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   grayish
_exptl_crystal_colour_primary    gray
_exptl_crystal_density_diffrn    1.939
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
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_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
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_refine_diff_density_max         2.336
_refine_diff_density_min         -1.539
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_restraints     0
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_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0738
_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^)+(0.1000P)^2^+50.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2102
_refine_ls_wR_factor_ref         0.2135
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6116
_reflns_number_total             6693
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02351k2.cif
_cod_data_source_block           gd
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               1546873
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H29 of C29, H12 of C12, H15 of C15, H16 of C16, H10 of C10, H6 of C6, {H11A,
  H11B} of C11, H14 of C14, {H9A,H9B} of C9, H5 of C5, H8 of C8, H24 of C24, H4
  of C4
 At 1.5 times of:
  {H19A,H19B,H19C} of C19, {H12A,H12B} of O12, H3 of O3, {H1A,H1B,H1C} of C1
2.a Rotating group:
 O12(H12A,H12B)
2.b Ternary CH refined with riding coordinates:
 C10(H10)
2.c Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B)
2.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C24(H24), C4(H4), C29(H29), C12(H12), C15(H15), C16(H16),
 C6(H6), C14(H14)
2.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C19(H19A,H19B,H19C)
2.f Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_res_checksum              3740
_shelx_shelxl_version_number     2014/7