Chiral six-coordinate Dy(III) and Tb(III) complexes of an achiral ligand: Structure, fluorescence, and magnetism
Liu, Mei-Jiao; Yuan, Juan; Zhang, Yiquan; Sun, Hao-Ling; Liu, Cai-Ming; Kou, Hui-Zhong; Dalton Trans.  (2017) –; doi:10.1039/C7DT02409F

data_7044170
_publ_section_title
;
 Chiral six-coordinate Dy(III) and Tb(III) complexes of an achiral ligand:
 Structure, fluorescence, and magnetism
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02409F
_journal_year                    2017
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C66 H90 Cl3 N6 O6 Tb Zn3, 1.5(O)'
_chemical_formula_sum            'C66 H93 Cl3 N6 O7.5 Tb Zn3'
_chemical_formula_weight         1551.84
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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     heavy
_audit_creation_date             2017-06-12
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-07-03 deposited with the CCDC.
2017-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                74.076(3)
_cell_angle_beta                 82.733(2)
_cell_angle_gamma                80.874(2)
_cell_formula_units_Z            2
_cell_length_a                   12.4384(4)
_cell_length_b                   16.3219(5)
_cell_length_c                   19.7909(6)
_cell_measurement_reflns_used    31917
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.3680
_cell_measurement_theta_min      4.3270
_cell_volume                     3800.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.982
_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     12.00  70.00   1.00    1.00    --   40.81  77.00  90.00   58
  2  \w     71.00 113.00   1.00    1.00    --   40.81  77.00  90.00   42
  3  \w     83.00 113.00   1.00    1.00    --   40.81  57.00 150.00   30
  4  \w     73.00  99.00   1.00    3.00    --  100.91  61.00  60.00   26
  5  \w    113.00 177.00   1.00    3.00    --  100.91  77.00  60.00   64
  6  \w    117.00 163.00   1.00    3.00    --  100.91  77.00 -60.00   46
  7  \w    147.00 173.00   1.00    3.00    --  100.91  77.00-120.00   26
  8  \w    106.00 173.00   1.00    3.00    --  100.91  77.00-180.00   67
  9  \w    106.00 176.00   1.00    3.00    --  100.91  77.00 -30.00   70
 10  \w     73.00 100.00   1.00    1.00    --   40.81  77.00-180.00   27
 11  \w     68.00  94.00   1.00    3.00    --  100.91  77.00-120.00   26
 12  \w     73.00 100.00   1.00    3.00    --  100.91  61.00-150.00   27
 13  \w     72.00  99.00   1.00    3.00    --  100.91  61.00-180.00   27
 14  \w     68.00  94.00   1.00    3.00    --  100.91  77.00-180.00   26
 15  \w     68.00  96.00   1.00    3.00    --  100.91  77.00-150.00   28
 16  \w     72.00 159.00   1.00    3.00    --  100.91  61.00-120.00   87
 17  \w     68.00 172.00   1.00    3.00    --  100.91  77.00  30.00  104
 18  \w     68.00 176.00   1.00    3.00    --  100.91  77.00 150.00  108
 19  \w     72.00 172.00   1.00    3.00    --  100.91  61.00 120.00  100
 20  \w     68.00 171.00   1.00    3.00    --  100.91  77.00 -90.00  103
 21  \w     72.00 113.00   1.00    3.00    --  100.91  61.00 -30.00   41
 22  \w     72.00  99.00   1.00    3.00    --  100.91  61.00   0.00   27
 23  \w     72.00 129.00   1.00    3.00    --  100.91  61.00  30.00   57
 24  \w     72.00  98.00   1.00    3.00    --  100.91  61.00 150.00   26
 25  \w     68.00 106.00   1.00    3.00    --  100.91  77.00  90.00   38
 26  \w     72.00 109.00   1.00    3.00    --  100.91  61.00  90.00   37
 27  \w     68.00  94.00   1.00    3.00    --  100.91  77.00  60.00   26
 28  \w     68.00  94.00   1.00    3.00    --  100.91  77.00 120.00   26
 29  \w     68.00  99.00   1.00    3.00    --  100.91  77.00   0.00   31
 30  \w     68.00  94.00   1.00    3.00    --  100.91  77.00 -60.00   26
 31  \w     68.00  94.00   1.00    3.00    --  100.91  77.00 -30.00   26
 32  \w      9.00  71.00   1.00    1.00    --   40.81  77.00-180.00   62
 33  \w      8.00 110.00   1.00    1.00    --   40.81  77.00-120.00  102
 34  \w      8.00  99.00   1.00    1.00    --   40.81  77.00 -60.00   91
 35  \w      9.00 117.00   1.00    1.00    --   40.81  77.00  30.00  108
 36  \w     13.00  63.00   1.00    1.00    --   40.81  57.00 150.00   50
 37  \w     30.00 133.00   1.00    3.00    --  100.91 -77.00  60.00  103
 38  \w     75.00 132.00   1.00    3.00    --  100.91 -77.00-150.00   57
 39  \w     33.00 109.00   1.00    3.00    --  100.91 -95.00   0.00   76
 40  \w     25.00  53.00   1.00    3.00    --  100.91 -77.00-150.00   28
 41  \w     28.00 120.00   1.00    3.00    --  100.91-125.00 -90.00   92
 42  \w      2.00  72.00   1.00    1.00    --   40.81 -99.00 -90.00   70
 43  \w    -69.00  30.00   1.00    1.00    --  -40.81  57.00-180.00   99
 44  \w    -69.00  29.00   1.00    1.00    --  -40.81  57.00  60.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1136799000
_diffrn_orient_matrix_UB_12      0.0252800000
_diffrn_orient_matrix_UB_13      0.0015300000
_diffrn_orient_matrix_UB_21      0.0530228000
_diffrn_orient_matrix_UB_22      -0.0714377000
_diffrn_orient_matrix_UB_23      -0.0354154000
_diffrn_orient_matrix_UB_31      -0.0110726000
_diffrn_orient_matrix_UB_32      0.0636931000
_diffrn_orient_matrix_UB_33      -0.0731199000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            58530
_diffrn_reflns_point_group_measured_fraction_full 0.929
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.503
_diffrn_reflns_theta_min         3.613
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.926
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51050
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       block
_exptl_crystal_F_000             1594
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.015(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1621
_refine_ls_number_reflns         26732
_refine_ls_number_restraints     760
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0619
_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^)+(0.1180P)^2^+2.3450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1662
_refine_ls_wR_factor_ref         0.1727
_reflns_Friedel_coverage         0.839
_reflns_Friedel_fraction_full    0.861
_reflns_Friedel_fraction_max     0.824
_reflns_number_gt                24564
_reflns_number_total             26732
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02409f3.cif
_cod_data_source_block           2-lambda
_cod_original_formula_sum        'C66 H93 Cl3 N6 O7.50 Tb Zn3'
_cod_database_code               7044170
_chemical_oxdiff_formula         CHNOTb
_chemical_oxdiff_usercomment     CHNOTb
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C77-C78
 1.453 with sigma of 0.005
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C20) \\sim Ueq, Uanis(O2W) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C72) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C10) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C77)
\\sim Ueq, Uanis(C100) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C6) \\sim Ueq,
Uanis(C104) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O3W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C98) \\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C5)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O6W) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O4W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: O1W(0.5) O2W(0.5) O3W(0.75) O4W(0.25) O5W(0.5) O6W(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C11(H11a,H11b), C12(H12a,H12b), C14(H14a,H14b), C31(H31a,H31b),
 C33(H33a,H33b), C34(H34a,H34b), C36(H36a,H36b), C53(H53a,H53b), C55(H55a,H55b),
  C56(H56a,H56b), C58(H58a,H58b), C75(H75a,H75b), C77(H77a,H77b), C78(H78a,
 H78b), C80(H80a,H80b), C97(H97a,H97b), C99(H99a,H99b), C100(H10d,H10e),
 C102(H10i,H10j), C119(H11i,H11j), C121(H12f,H12g), C122(H12h,H12i), C124(H12m,
 H12n)
6.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C16(H16), C21(H21), C23(H23), C28(H28), C37(H37), C41(H41),
 C46(H46), C51(H51), C60(H60), C65(H65), C68(H68), C73(H73), C82(H82), C87(H87),
  C90(H90), C95(H95), C104(H104), C109(H109), C112(H112), C117(H117),
 C126(H126), C131(H131)
6.c Idealised Me refined as rotating group:
 C3(H3a,H3b,H3c), C5(H5a,H5b,H5c), C10(H10a,H10b,H10c), C13(H13a,H13b,H13c),
 C18(H18a,H18b,H18c), C20(H20a,H20b,H20c), C25(H25a,H25b,H25c), C27(H27a,H27b,
 H27c), C32(H32a,H32b,H32c), C35(H35a,H35b,H35c), C39(H39a,H39b,H39c), C44(H44a,
 H44b,H44c), C48(H48a,H48b,H48c), C50(H50a,H50b,H50c), C54(H54a,H54b,H54c),
 C57(H57a,H57b,H57c), C62(H62a,H62b,H62c), C64(H64a,H64b,H64c), C70(H70a,H70b,
 H70c), C72(H72a,H72b,H72c), C76(H76a,H76b,H76c), C79(H79a,H79b,H79c), C84(H84a,
 H84b,H84c), C86(H86a,H86b,H86c), C92(H92a,H92b,H92c), C94(H94a,H94b,H94c),
 C98(H98a,H98b,H98c), C101(H10f,H10g,H10h), C106(H10k,H10l,H10m), C108(H10n,
 H10o,H10p), C114(H11c,H11d,H11e), C116(H11f,H11g,H11h), C120(H12c,H12d,H12e),
 C123(H12j,H12k,H12l), C128(H12o,H12p,H12q), C130(H13d,H13e,H13f)
;
_shelx_shelxl_version_number     2014/7
_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 1.682
_oxdiff_exptl_absorpt_empirical_full_min 0.676