Enhanced near-infrared luminescence in Ln2Cd2 (Ln = Nd, Yb) heterotetranuclear complexes
Qi, Yue; Sun, Ou; Zhou, Yanyan; Yao, Yuan; Cheng, Zhenyu; Gao, Ting; Li, Hongfeng; CrystEngComm  (2020) –; doi:10.1039/D0CE00341G

data_7240272
_publ_section_title
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 Enhanced near-infrared luminescence in Ln2Cd2 (Ln = Nd, Yb)
 heterotetranuclear complexes
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_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00341G
_journal_year                    2020
_chemical_formula_moiety         'C82 H66 Cd2 F12 N4 Nd2 O22 S4, 4(C H2 Cl2)'
_chemical_formula_sum            'C86 H74 Cd2 Cl8 F12 N4 Nd2 O22 S4'
_chemical_formula_weight         2668.61
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-10-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-11 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                88.674(2)
_cell_angle_beta                 81.057(3)
_cell_angle_gamma                77.969(2)
_cell_formula_units_Z            1
_cell_length_a                   10.7102(8)
_cell_length_b                   12.4241(9)
_cell_length_c                   18.9297(14)
_cell_measurement_reflns_used    9782
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      3.15
_cell_volume                     2433.5(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_unetI/netI     0.0090
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            127756
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.92
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.880
_exptl_absorpt_correction_T_max  0.8343
_exptl_absorpt_correction_T_min  0.7657
_exptl_crystal_density_diffrn    1.821
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1318
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.263
_refine_diff_density_min         -2.426
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         12059
_refine_ls_number_restraints     207
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0622P)^2^+17.4150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1321
_refine_ls_wR_factor_ref         0.1346
_reflns_number_gt                11470
_reflns_number_total             12059
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0ce00341g2.cif
_cod_data_source_block           c
_cod_database_code               7240272
_olex2_refinement_description
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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, All O(H) groups
2. Restrained distances
 O9-H9
 0.87 with sigma of 0.01
 C25-H9
 1.886488 with sigma of 0.02
 Cd1-H9
 2.987502 with sigma of 0.02
 F4-F5 \\sim F5-F6 \\sim F6-F4 \\sim F4'-F5' \\sim F5'-F6' \\sim F6'-F4'
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl4) \\sim Ueq, Uanis(Cl3) \\sim Ueq, Uanis(Cl3') \\sim Ueq, Uanis(Cl4')
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(Cl1) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(Cl3) \\sim Ueq, Uanis(Cl4)
\\sim Ueq, Uanis(Cl1') \\sim Ueq, Uanis(Cl2') \\sim Ueq, Uanis(Cl3') \\sim Ueq,
Uanis(Cl4') \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C42')
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C39) = Uanis(S2) = Uanis(S2') = Uanis(C39')
Uanis(F4) = Uanis(F5) = Uanis(F6) = Uanis(F4') = Uanis(F5') = Uanis(F6')
Uanis(Cl1) = Uanis(Cl1')
Uanis(Cl2) = Uanis(Cl2')
Uanis(Cl3) = Uanis(Cl3')
Uanis(Cl4) = Uanis(Cl4')
Uanis(C42) = Uanis(C42')
4. Others
 Sof(Cl4')=Sof(Cl3')=1-FVAR(1)
 Sof(Cl4)=Sof(Cl3)=FVAR(1)
 Sof(S2')=Sof(C39')=Sof(H39B)=1-FVAR(2)
 Sof(S2)=Sof(C39)=Sof(H39A)=FVAR(2)
 Sof(F4')=Sof(F5')=Sof(F6')=1-FVAR(3)
 Sof(F4)=Sof(F6)=Sof(F5)=FVAR(3)
 Sof(Cl2')=Sof(C42')=Sof(H42A)=Sof(H42B)=Sof(Cl1')=1-FVAR(4)
 Sof(C42)=Sof(H42C)=Sof(H42D)=Sof(Cl2)=Sof(Cl1)=FVAR(4)
5.a Riding coordinates:
 C39(H39A), C39'(H39B), C40(H40), C41(H41), O9(H9)
5.b Secondary CH2 refined with riding coordinates:
 C42'(H42A,H42B), C42(H42C,H42D)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C11(H11), C13(H13), C14(H14),
 C15(H15), C17(H17), C18(H18), C19(H19), C28(H28), C31(H31A), C32(H32),
 C33(H33), C36(H36)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C)
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_olex2_submission_special_instructions 'No special instructions were received'