Four Salamo-type 3d-4f hetero-bimetallic [ZnIILnIII] complexes: Syntheses, Crystal Structures, Luminescent and Magnetic Properties
Zheng, Shan shan; Dong, WK; Zhang, Yang; Chen, Le; Ding, Yujie; New J. Chem. 41 (2017) 4966–4973; doi:10.1039/C6NJ04090J

data_7056171
_publ_section_title
;
 Four Salamo-type 3d-4f hetero-bimetallic [ZnIILnIII] complexes:
 Syntheses, Crystal Structures, Luminescent and Magnetic Properties
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              4966
_journal_page_last               4973
_journal_paper_doi               10.1039/C6NJ04090J
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C22 H25 N4 O14 Tb Zn'
_chemical_formula_sum            'C22 H25 N4 O14 Tb Zn'
_chemical_formula_weight         793.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-12-23 deposited with the CCDC.
2017-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.340(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1130(6)
_cell_length_b                   13.2655(5)
_cell_length_c                   16.3649(7)
_cell_measurement_reflns_used    2705
_cell_measurement_temperature    298.84(10)
_cell_measurement_theta_max      27.3570
_cell_measurement_theta_min      3.4900
_cell_volume                     2758.0(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
;
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, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.84(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -90.00  -50.10   1.0500    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3492  -57.0000   30.0000 38

  2 omega  -37.00   39.65   1.0500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6305  -77.0000  120.0000 73

  3 omega   -9.00   96.00   1.0500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6305   38.0000  -90.0000 100

  4 omega   -6.00   23.40   1.0500    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3492  -99.0000 -150.0000 28
;
_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      -0.0028811000
_diffrn_orient_matrix_UB_12      -0.0531925000
_diffrn_orient_matrix_UB_13      -0.0046655000
_diffrn_orient_matrix_UB_21      0.0539606000
_diffrn_orient_matrix_UB_22      -0.0014294000
_diffrn_orient_matrix_UB_23      -0.0003397000
_diffrn_orient_matrix_UB_31      0.0140254000
_diffrn_orient_matrix_UB_32      -0.0054897000
_diffrn_orient_matrix_UB_33      0.0444754000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0708
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11153
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         3.329
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.490
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97595
_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.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.912
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.900
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         5419
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0140P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4078
_reflns_number_total             5419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj04090j2.cif
_cod_data_source_block           d954
_cod_database_code               7056171
_reflns_odcompleteness_completeness 99.70
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H19A(0.5) H19B(0.5) H19C(0.5) H19D(0.5) C20(0.5) H20A(0.5)
 H20B(0.5) H20C(0.5) C20'(0.5) H20D(0.5) H20E(0.5) H20F(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C10(H10A,H10B), C11(H11A,H11B), C19(H19A,H19B), C19(H19C,H19D)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C12(H12), C14(H14), C15(H15), C16(H16)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3AA(H3AA,H3AB,H3AC), C20(H20A,H20B,H20C), C20'(H20D,H20E,
 H20F)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-07-11
_olex2_submission_special_instructions 'No special instructions were received'