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_1546866
_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 Dy F15 N2 Ni O12'
_chemical_formula_sum            'C31 H24 Dy F15 N2 Ni O12'
_chemical_formula_weight         1122.73
_chemical_name_systematic
;
 ? 
;
_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             2017-07-31
_audit_creation_method
;
  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                 97.946(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2854(7)
_cell_length_b                   12.6822(4)
_cell_length_c                   16.6662(5)
_cell_measurement_reflns_used    4656
_cell_measurement_temperature    128.45(10)
_cell_measurement_theta_max      27.9180
_cell_measurement_theta_min      3.4220
_cell_volume                     3827.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      128.45(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9979
_diffrn_measured_fraction_theta_max 0.9979
_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    -50.00  14.00   1.00    5.50    --   18.94 -57.00 -30.00   64
  2  \w    -47.00  54.00   1.00    5.50    --  -19.25  19.00 150.00  101
  3  \w     63.00  95.00   1.00    5.50    --   18.94 178.00  30.00   32
  4  \w     54.00  87.00   1.00    5.50    --   18.94 178.00-180.00   33
  5  \w    -83.00 -51.00   1.00    5.50    --  -19.25 -57.00  30.00   32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0320519000
_diffrn_orient_matrix_UB_12      -0.0284926000
_diffrn_orient_matrix_UB_13      0.0161325000
_diffrn_orient_matrix_UB_21      0.0207862000
_diffrn_orient_matrix_UB_22      0.0272755000
_diffrn_orient_matrix_UB_23      -0.0264098000
_diffrn_orient_matrix_UB_31      0.0088042000
_diffrn_orient_matrix_UB_32      0.0395845000
_diffrn_orient_matrix_UB_33      0.0297961000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16229
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.945
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.565
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear grayish gray'
_exptl_crystal_density_diffrn    1.948
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2196
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_transmission_factor_max   0.2
_exptl_transmission_factor_min   0.1
_refine_diff_density_max         1.633
_refine_diff_density_min         -1.335
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         6729
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0609
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+40.4167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1188
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5068
_reflns_number_total             6729
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02351k2.cif
_cod_data_source_block           p20160601e
_cod_database_code               1546866
_chemical_oxdiff_formula         NiDyCHONFCl
_chemical_oxdiff_usercomment     JiangNiDy
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H9A,H9B} of C9, H5 of C5, H4 of C4, H8 of C8, H15 of C15, H10 of C10, H29
  of C29, {H11A,H11B} of C11, H14 of C14, H12 of C12, H16 of C16, H6 of C6, H24
  of C24
 At 1.5 times of:
  {H1A,H1B,H1C} of C1, {H12A,H12B} of O12, {H19A,H19B,H19C} of C19, H3 of O3
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:
 C14(H14), C12(H12), C16(H16), C6(H6), C24(H24), C5(H5), C4(H4), C8(H8),
 C15(H15), C29(H29)
2.e Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C1(H1A,H1B,H1C)
2.f Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_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 1.132
_oxdiff_exptl_absorpt_empirical_full_min 0.891
_shelx_res_checksum              87928
_shelx_shelxl_version_number     2014/7