Polymorphism modulates photoluminescence and magnetic dynamics of mononuclear dysprosium-anthracene complexes
Ma, XiuFang; Guo, Ying; Huang, Xin-Da; Wen, Ge-Hua; Bao, Song-Song; Zhang, Yi-Quan; Zheng, Li-Min; Dalton Transactions  (2022) –; doi:10.1039/D2DT01710E

data_7710701
_publ_section_title
;
 Polymorphism modulates photoluminescence and magnetic dynamics of
 mononuclear dysprosium-anthracene complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01710E
_journal_year                    2022
_chemical_formula_moiety         'C57 H63 Br3 Dy O9 P3'
_chemical_formula_sum            'C57 H63 Br3 Dy O9 P3'
_chemical_formula_weight         1387.21
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-04-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2022-04-27 deposited with the CCDC.	2022-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                80.018(6)
_cell_angle_beta                 85.631(7)
_cell_angle_gamma                80.695(6)
_cell_formula_units_Z            2
_cell_length_a                   10.876(4)
_cell_length_b                   12.003(5)
_cell_length_c                   23.079(9)
_cell_measurement_reflns_used    6220
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.1325
_cell_measurement_theta_min      2.376
_cell_volume                     2925(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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_temperature      296.15
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0758
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            22574
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.385
_diffrn_reflns_theta_min         1.743
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.461
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_description       block
_exptl_crystal_F_000             1386
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.480
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         10339
_refine_ls_number_restraints     271
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0622P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1110
_refine_ls_wR_factor_ref         0.1251
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7303
_reflns_number_total             10339
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01710e2.cif
_cod_data_source_block           y
_cod_original_cell_volume        2924.9(19)
_cod_database_code               7710701
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.7452
_shelx_estimated_absorpt_t_min   0.5925
_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. Restrained distances
 C56-C57
 1.5 with sigma of 0.01
 C54-C55
 1.5 with sigma of 0.01
 C36-C35
 1.5 with sigma of 0.01
 C57-C56
 1.5 with sigma of 0.005
 C57B-C56
 1.5 with sigma of 0.005
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C19)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(C35) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C38) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C36) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=Sof(H56C)=Sof(H56D)=1-FVAR(1)
 Sof(H56A)=Sof(H56B)=Sof(C57B)=Sof(H57D)=Sof(H57E)=Sof(H57F)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C1(H1A,H1B), C39(H39A,H39B), C35(H35A,H35B), C54(H54A,H54B),
 C16(H16A,H16B), C18(H18A,H18B), C37(H37A,H37B), C56(H56C,H56D), C56(H56A,H56B)
6.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C31(H31), C11(H11), C23(H23), C44(H44), C52(H52), C33(H33),
 C28(H28), C49(H49), C50(H50), C43(H43), C47(H47), C30(H30), C12(H12), C4(H4),
 C26(H26), C51(H51), C45(H45), C9(H9), C32(H32), C42(H42), C7(H7), C13(H13),
 C25(H25), C24(H24), C5(H5), C6(H6)
6.c Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C38(H38A,H38B,H38C), C57(H57A,H57B,H57C), C19(H19A,H19B,
 H19C), C57B(H57D,H57E,H57F), C36(H36A,H36B,H36C), C17(H17A,H17B,H17C)
;
_olex2_submission_special_instructions 'No special instructions were received'