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_7056170
_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 Dy N4 O14 Zn'
_chemical_formula_sum            'C22 H25 Dy N4 O14 Zn'
_chemical_formula_weight         797.33
_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)
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_audit_update_record
;
2016-12-23 deposited with the CCDC.
2017-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.270(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0950(5)
_cell_length_b                   13.2699(4)
_cell_length_c                   16.3621(6)
_cell_measurement_reflns_used    3184
_cell_measurement_temperature    298.84(10)
_cell_measurement_theta_max      27.5140
_cell_measurement_theta_min      3.5460
_cell_volume                     2755.50(17)
_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  -95.00  -55.10   1.0500    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.5055  178.0000   60.0000 38

  2 omega   -8.00   58.15   1.0500    2.5000
omega____ theta____ kappa____ phi______ frames
    -       22.7867  -99.0000  -60.0000 63

  3 omega  -34.00   88.85   1.0500    2.5000
omega____ theta____ kappa____ phi______ frames
    -       22.7867  -19.0000  -30.0000 117
;
_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      0.0253774000
_diffrn_orient_matrix_UB_12      0.0334212000
_diffrn_orient_matrix_UB_13      -0.0224621000
_diffrn_orient_matrix_UB_21      0.0459291000
_diffrn_orient_matrix_UB_22      -0.0010149000
_diffrn_orient_matrix_UB_23      0.0337593000
_diffrn_orient_matrix_UB_31      0.0192277000
_diffrn_orient_matrix_UB_32      -0.0417107000
_diffrn_orient_matrix_UB_33      -0.0188902000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0582
_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       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10368
_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         3.465
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.638
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92873
_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    1.922
_exptl_crystal_description       block
_exptl_crystal_F_000             1572
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         5413
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0150P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0642
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4317
_reflns_number_total             5413
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj04090j2.cif
_cod_data_source_block           d955
_cod_original_cell_volume        2755.52(17)
_cod_database_code               7056170
_reflns_odcompleteness_completeness 99.71
_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) C1(0.5) H1A(0.5) H1B(0.5)
 H1C(0.5) C2(0.5) H2A(0.5) H2B(0.5) H2C(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C3AA(H3AA,H3AB), C10(H10A,H10B), C11(H11A,H11B), C19(H19A,H19B), C19(H19C,H19D)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C9(H9), C12(H12), C16(H16), C17(H17), C18(H18)
3.c Idealised Me refined as rotating group:
 C0AA(H0AA,H0AB,H0AC), C21(H21A,H21B,H21C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-07-12
_olex2_submission_special_instructions 'No special instructions were received'