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_1546877
_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         'C66 H57 Cl4 Ho N2 Ni O11'
_chemical_formula_sum            'C66 H57 Cl4 Ho N2 Ni O11'
_chemical_formula_weight         1419.56
_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             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                81.822(3)
_cell_angle_beta                 83.284(3)
_cell_angle_gamma                76.675(3)
_cell_formula_units_Z            2
_cell_length_a                   11.2770(4)
_cell_length_b                   12.6970(5)
_cell_length_c                   23.3931(8)
_cell_measurement_reflns_used    11845
_cell_measurement_temperature    128.75(10)
_cell_measurement_theta_max      28.8560
_cell_measurement_theta_min      3.2390
_cell_volume                     3213.9(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-1997 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      128.75(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.6107
_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    -17.00  92.00   1.00    7.00    --   18.94  19.00-120.00  109
  2  \w      1.00  60.00   1.00    7.00    --   18.94 -99.00-120.00   59
  3  \w     24.00  61.00   1.00    7.00    --   18.94 -99.00 120.00   37
  4  \w    -42.00  50.00   1.00    7.00    --  -19.25  77.00  60.00   92
  5  \w    -82.00  11.00   1.00    7.00    --  -19.25 -77.00 -60.00   93
  6  \w    -89.00 -64.00   1.00    7.00    --  -19.25-178.00 150.00   25
;
_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      0.0472782000
_diffrn_orient_matrix_UB_12      -0.0423244000
_diffrn_orient_matrix_UB_13      -0.0100710000
_diffrn_orient_matrix_UB_21      0.0347001000
_diffrn_orient_matrix_UB_22      0.0389373000
_diffrn_orient_matrix_UB_23      -0.0123469000
_diffrn_orient_matrix_UB_31      0.0277656000
_diffrn_orient_matrix_UB_32      -0.0059880000
_diffrn_orient_matrix_UB_33      0.0262993000
_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  0.0424
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22961
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         3.046
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.741
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80408
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       prism
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.042
_refine_diff_density_min         -1.025
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     780
_refine_ls_number_reflns         11450
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+3.8928P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0902
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10319
_reflns_number_total             11450
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02351k2.cif
_cod_data_source_block           p160615h_sq
_cod_database_code               1546877
_chemical_oxdiff_formula         CHONNiHoCl
_chemical_oxdiff_usercomment     jianglinNiHo
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H6 of C6, H8 of C8, H5 of C5, H33 of C33, H23 of C23, H4 of C4, {H11A,H11B}
  of C11, H54 of C54, H15 of C15, {H9A,H9B} of C9, H32 of C32, H30 of C30, H61
  of C61, H62 of C62, H31 of C31, {H68A,H68B} of C68, {H67A,H67B,H67C,H67D} of
  C67, H27 of C27, H49 of C49, H47 of C47, H36 of C36, H53 of C53, H25 of C25,
  H24 of C24, H37 of C37, H42 of C42, H10 of C10, H14 of C14, H55 of C55, H26
  of C26, H57 of C57, H46 of C46, H22 of C22, H63 of C63, H40 of C40, H39 of
  C39, H52 of C52, H48 of C48, H34 of C34, H51 of C51, H38 of C38, H65 of C65,
  H45 of C45, H16 of C16, H60 of C60, H12 of C12
 At 1.5 times of:
  {H1A,H1B,H1C} of C1, H3 of O3, {H19A,H19B,H19C} of C19
2. Others
 1-Sof(H67B)=1-Sof(H67B)=Sof(H67C)=Sof(H67D)
 1-Sof(Cl2B)=Sof(Cl2B)
3.a Ternary CH refined with riding coordinates:
 C10(H10)
3.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C9(H9A,H9B), C68(H68A,H68B), C67(H67A,H67B), C67(H67C,H67D)
3.c Aromatic/amide H refined with riding coordinates:
 C42(H42), C37(H37), C24(H24), C25(H25), C53(H53), C36(H36), C47(H47),
 C49(H49), C27(H27), C22(H22), C63(H63), C40(H40), C39(H39), C52(H52), C48(H48),
  C34(H34), C51(H51), C38(H38), C65(H65), C45(H45), C16(H16), C60(H60),
 C12(H12), C46(H46), C57(H57), C26(H26), C55(H55), C14(H14), C6(H6), C8(H8),
 C5(H5), C33(H33), C23(H23), C4(H4), C54(H54), C15(H15), C32(H32), C30(H30),
 C61(H61), C62(H62), C31(H31)
3.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C1(H1A,H1B,H1C)
3.e 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 1.300
_oxdiff_exptl_absorpt_empirical_full_min 0.712
_shelx_fab_checksum              93788
_shelx_res_checksum              30273
_shelx_shelxl_version_number     2014/7