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_7044171
_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, O'
_chemical_formula_sum            'C66 H92 Cl3 N6 O7 Tb Zn3'
_chemical_formula_weight         1542.83
_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     direct
_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                74.718(2)
_cell_angle_beta                 82.879(2)
_cell_angle_gamma                81.239(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3376(3)
_cell_length_b                   16.2163(4)
_cell_length_c                   19.4135(5)
_cell_measurement_reflns_used    27456
_cell_measurement_temperature    100.2(9)
_cell_measurement_theta_max      28.5280
_cell_measurement_theta_min      3.7980
_cell_volume                     3688.67(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7e (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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.2(9)
_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 0.885
_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    -59.00  26.00   1.00   21.84    --    9.97 -38.00 120.00   85
  2  \w    -20.00  51.00   1.00   21.84    --    9.97 -99.00-120.00   71
  3  \w    -15.00  81.00   1.00   21.84    --    9.97  38.00 -60.00   96
  4  \w    -20.00  86.00   1.00   21.84    --    9.97  77.00  30.00  106
  5  \w    -15.00  84.00   1.00   21.84    --    9.97  38.00-180.00   99
  6  \w    -88.00 -39.00   1.00   21.84    --  -11.85 154.00-162.94   49
  7  \w    -36.00  56.00   1.00   21.84    --  -11.85  38.00  30.00   92
  8  \w    -88.00 -42.00   1.00   21.84    --  -11.85 154.00  48.59   46
  9  \w    -88.00 -56.00   1.00   21.84    --  -11.85 154.00 -42.71   32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0272806000
_diffrn_orient_matrix_UB_12      0.0164049000
_diffrn_orient_matrix_UB_13      0.0226548000
_diffrn_orient_matrix_UB_21      0.0513007000
_diffrn_orient_matrix_UB_22      -0.0195436000
_diffrn_orient_matrix_UB_23      -0.0126909000
_diffrn_orient_matrix_UB_31      0.0058426000
_diffrn_orient_matrix_UB_32      0.0379164000
_diffrn_orient_matrix_UB_33      -0.0277789000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            68370
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.827
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.573
_diffrn_reflns_theta_min         3.287
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.070
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7e (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    1.389
_exptl_crystal_description       plate
_exptl_crystal_F_000             1584
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.382
_refine_diff_density_min         -1.157
_refine_diff_density_rms         0.141
_refine_ls_abs_structure_details
;
 Flack x determined using 10986 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(5)
_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     1594
_refine_ls_number_reflns         34214
_refine_ls_number_restraints     296
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0623
_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^)+(0.0635P)^2^+11.4748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1405
_refine_ls_wR_factor_ref         0.1507
_reflns_Friedel_coverage         0.868
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.768
_reflns_number_gt                29069
_reflns_number_total             34214
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02409f3.cif
_cod_data_source_block           2-delta
_cod_original_cell_volume        3688.67(17)
_cod_database_code               7044171
_chemical_oxdiff_formula         CHNOZnTbCl
_reflns_odcompleteness_completeness 99.77
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N7-C76
 1.5 with sigma of 0.005
 N3-C123 = N4-C10
 1.501 with sigma of 0.005
 C123-C10
 1.421 with sigma of 0.005
 C77-C78
 1.422 with sigma of 0.01
 C78-N8
 1.446 with sigma of 0.01
 C76-C77
 2.446 with sigma of 0.01
3. Rigid bond restraints
 C77, C78
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C54, C55
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N8, C78, C82, C83
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N4 \\sim C10: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C122) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C115)
\\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(N11) \\sim Ueq, Uanis(C31) \\sim Ueq,
Uanis(C76) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(N8) \\sim
Ueq, Uanis(C78) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C79) \\sim Ueq,
Uanis(O3W) \\sim Ueq, Uanis(C123) \\sim Ueq, Uanis(C124) \\sim Ueq, Uanis(C128)
\\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(O1W) \\sim Ueq,
Uanis(O2W) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C6) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C10)
\\sim Ueq, Uanis(C116) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C11) \\sim Ueq, Uanis(C121) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C128)
\\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C79) \\sim Ueq,
Uanis(C120) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C76) \\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C84)
\\sim Ueq, Uanis(C127) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C130) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C128) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C18)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C126)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: O2W(0.5) O3W(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C12(H12A,H12B), C30(H30A,H30B), C32(H32A,H32B), C33(H33A,
 H33B), C35(H35A,H35B), C52(H52A,H52B), C54(H54A,H54B), C55(H55A,H55B),
 C57(H57A,H57B), C65(H65A,H65B), C123(H12C,H12D), C75(H75A,H75B), C77(H77A,
 H77B), C78(H78A,H78B), C80(H80A,H80B), C97(H97A,H97B), C99(H99A,H99B),
 C100(H10C,H10D), C102(H10H,H10I), C119(H11J,H11K), C121(H12H,H12I), C122(H12J,
 H12K), C124(H12L,H12M)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C14(H14), C19(H19), C23(H23), C28(H28), C37(H37), C42(H42),
 C45(H45), C50(H50), C59(H59), C63(H63), 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:
 C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C25(H25A,H25B,H25C), C27(H27A,H27B,
 H27C), C31(H31A,H31B,H31C), C34(H34A,H34B,H34C), C39(H39A,H39B,H39C), C41(H41A,
 H41B,H41C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C53(H53A,H53B,H53C),
 C56(H56A,H56B,H56C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C), C0AA(H0AA,H0AB,
 H0AC), 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(H10E,H10F,H10G), C106(H10J,H10K,
 H10L), C108(H10M,H10N,H10O), C114(H11D,H11E,H11F), C116(H11G,H11H,H11I),
 C120(H12E,H12F,H12G), C128(H12N,H12O,H12P), C130(H13A,H13B,H13C)
;
_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 2.333
_oxdiff_exptl_absorpt_empirical_full_min 0.569