Programmable Photoluminescence via Intrinsic and DNA-Fluorophore Association in a Mixed Cluster Heterometallic MOF.
Sava Gallis, Dorina F.; Butler, Kimberly S.; Pearce, Charles J.; Valdez, Nichole; Rodriguez, Mark A.; ACS applied materials & interfaces 14 (2022) 10566–10576; doi:10.1021/acsami.1c24477

data_4519320
_publ_section_title
;
 Programmable Photoluminescence via Intrinsic and DNA-Fluorophore
 Association in a Mixed Cluster Heterometallic MOF.
;
_journal_issue                   8
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              10566
_journal_page_last               10576
_journal_paper_doi               10.1021/acsami.1c24477
_journal_volume                  14
_journal_year                    2022
_chemical_formula_moiety         'C138 Nd6 O64 Yb6'
_chemical_formula_sum            'C138 Nd6 O64 Yb6'
_chemical_formula_weight         4585.06
_space_group_crystal_system      trigonal
_space_group_IT_number           143
_space_group_name_Hall           'P 3'
_space_group_name_H-M_alt        'P 3'
_audit_creation_date             2020-07-20
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   40.2698(10)
_cell_length_b                   40.2698(10)
_cell_length_c                   23.9273(10)
_cell_measurement_reflns_used    9740
_cell_measurement_temperature    275.0
_cell_measurement_theta_max      65.22
_cell_measurement_theta_min      2.24
_cell_volume                     33603.4(18)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      275.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1322
_diffrn_reflns_av_unetI/netI     0.0984
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            417777
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        65.084
_diffrn_reflns_theta_max         65.084
_diffrn_reflns_theta_min         1.846
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.666
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1355 before and 0.0810 after correction.
The Ratio of minimum to maximum transmission is 0.8078.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.680
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             6360
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.349
_refine_diff_density_min         -1.995
_refine_diff_density_rms         0.284
_refine_ls_abs_structure_details
;
 Flack x determined using 14694 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.496(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     772
_refine_ls_number_reflns         76373
_refine_ls_number_restraints     197
_refine_ls_restrained_S_all      1.211
_refine_ls_R_factor_all          0.1833
_refine_ls_R_factor_gt           0.1084
_refine_ls_shift/su_max          5.009
_refine_ls_shift/su_mean         0.154
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3154
_refine_ls_wR_factor_ref         0.3743
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                41163
_reflns_number_total             76373
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am1c24477_si_002.cif
_cod_data_source_block           20_0407_17_b
_cod_original_cell_volume        33603(2)
_cod_database_code               4519320
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 C114-C117
 1.54 with sigma of 0.02
 C144-C147
 1.54 with sigma of 0.02
 C214-C217
 1.54 with sigma of 0.02
 C324-C327
 1.54 with sigma of 0.02
 C334-C337
 1.54 with sigma of 0.02
 C414-C417
 1.54 with sigma of 0.02
 C424-C427
 1.54 with sigma of 0.02
 C444-C447
 1.54 with sigma of 0.02
 C244-C247
 0.02 with sigma of 1.54
 C264-C267
 0.02 with sigma of 1.54
 C364-C367
 0.01 with sigma of 1.54
 C113-C117 \\sim C115-C117
 with sigma of 0.02
 C120-C111 \\sim C160-C111
 with sigma of 0.02
 C143-C147 \\sim C145-C147
 with sigma of 0.02
 C213-C217 \\sim C215-C217
 with sigma of 0.02
 C323-C327 \\sim C325-C327
 with sigma of 0.02
 C413-C417 \\sim C415-C417
 with sigma of 0.02
 C423-C427 \\sim C425-C427
 with sigma of 0.02
 C427-O427 \\sim C427-O428
 with sigma of 0.02
 C443-C447 \\sim C445-C447
 with sigma of 0.02
 C447-O447 \\sim C447-O448
 with sigma of 0.02
 C453-C457 \\sim C455-C457
 with sigma of 0.02
 O2A-Nd2A \\sim O2A-Nd3A
 with sigma of 0.02
 O2B-Nd2B \\sim O2B-Nd3B
 with sigma of 0.02
 O2A-Nd2A \\sim O2B-Nd2B
 with sigma of 0.02
 O2B-Nd3A \\sim O2B-Nd3B
 with sigma of 0.02
 O5A-Nd4A \\sim O5A-Nd5A
 with sigma of 0.02
 O5B-Nd4B \\sim O5B-Nd5B
 with sigma of 0.02
 O5A-Nd4A \\sim O5B-Nd4B
 with sigma of 0.02
 O5A-Nd5A \\sim O5B-Nd5B
 with sigma of 0.02
 O5A-Nd5A \\sim O2B-Nd3B
 with sigma of 0.02
 O5A-Nd4A \\sim O2B-Nd3B
 with sigma of 0.02
 O5B-Nd5B \\sim O2A-Nd2A
 with sigma of 0.02
 O5B-Nd4B \\sim O2A-Nd3A
 with sigma of 0.02
 C11-O111 \\sim C11-O112
 with sigma of 0.02
 C12-O121 \\sim C12-O122
 with sigma of 0.02
 Yb1-O111 \\sim Yb2-O112
 with sigma of 0.02
 Yb4-O122 \\sim Yb3-O121
 with sigma of 0.02
 Yb1-O111 \\sim Yb4-O122
 with sigma of 0.02
 Yb2-O112 \\sim Yb3-O121
 with sigma of 0.02
 O2B-Nd1B \\sim O2B-Nd2B
 with sigma of 0.02
 O2B-Nd1B \\sim O2B-Nd3B
 with sigma of 0.02
 O3B-Nd3B \\sim O3B-Nd2B
 with sigma of 0.02
 O3B-Nd3B \\sim O3B-Nd5B
 with sigma of 0.02
 O4B-Nd4B \\sim O4B-Nd2B
 with sigma of 0.02
 O4B-Nd4B \\sim O4B-Nd3B
 with sigma of 0.02
 O2A-Nd1A \\sim O2A-Nd2A
 with sigma of 0.02
 O2A-Nd1A \\sim O2A-Nd3A
 with sigma of 0.02
 O3A-Nd3A \\sim O3A-Nd5A
 with sigma of 0.02
 O3A-Nd3A \\sim O3A-Nd4A
 with sigma of 0.02
 O4A-Nd2A \\sim O4A-Nd4A
 with sigma of 0.02
 O4A-Nd2A \\sim O4A-Nd5A
 with sigma of 0.02
 C127-O127 \\sim C127-O128
 with sigma of 0.02
 C243-C247 \\sim C245-C247
 with sigma of 0.02
 O247-C247 \\sim O248-C247
 with sigma of 0.02
 C263-C267 \\sim C265-C267
 with sigma of 0.02
 O267-C267 \\sim O268-C267
 with sigma of 0.02
 C363-C367 \\sim C365-C367
 with sigma of 0.02
 O367-C367 \\sim O368-C367
 with sigma of 0.02
 C350-C361 \\sim C310-C361
 with sigma of 0.02
 C121-C110 \\sim C121-C130
 with sigma of 0.02
 C237-O237 \\sim C237-O238
 with sigma of 0.02
 Nd1A-O10A \\sim Nd1B-O10B
 with sigma of 0.02
 C327-O327 \\sim C327-O328
 with sigma of 0.02
 Nd5A-O53 \\sim Nd5A-O5
 with sigma of 0.02
 Nd5A-O11A \\sim Nd4A-O12A
 with sigma of 0.02
 Nd2B-O12B \\sim Nd3B-O11B
 with sigma of 0.02
2. Restrained planarity
 C12, O121, O122, Yb4, Yb3
 with sigma of 0.1
 C110, C120, C160, C111
 with sigma of 0.1
 C110, C111, C112, C113, C114, C115, C116, C117
 with sigma of 0.04
 C110, C120, C130, C140, C150, C160, C111, C121, C151
 with sigma of 0.04
 C210, C220, C230, C240, C250, C260, C211, C231, C241, C261
 with sigma of 0.04
 C310, C320, C330, C340, C350, C360, C331, C351, C361
 with sigma of 0.04
 C410, C420, C430, C440, C450, C460, C411, C421, C441
 with sigma of 0.04
 C143, C144, C145, C147
 with sigma of 0.1
 C213, C214, C215, C217
 with sigma of 0.1
 C231, C232, C235, C236
 with sigma of 0.1
 C323, C324, C325, C327
 with sigma of 0.1
 C413, C414, C415, C417
 with sigma of 0.1
 C423, C424, C425, C427
 with sigma of 0.1
 C440, C450, C460, C441
 with sigma of 0.1
 C443, C444, C445, C447
 with sigma of 0.1
 C453, C454, C455, C457
 with sigma of 0.1
 Nd1A, Nd1B, O2A, O2B, O5A, O5B, Nd6A, Nd6B
 with sigma of 0.05
 C353, C354, C355, C357
 with sigma of 0.1
 C243, C244, C245, C247
 with sigma of 0.1
 C263, C264, C265, C267
 with sigma of 0.1
 O267, C267, O268, C267
 with sigma of 0.1
 C363, C364, C365, C367
 with sigma of 0.1
 C110, C120, C130, C121
 with sigma of 0.1
 C237, O237, C237, O238
 with sigma of 0.1
 C324, C327, O327, O328
 with sigma of 0.1
 C264, C267, O267, O268
 with sigma of 0.1
 C150, C151, C152, C153, C154, C155, C156, C120, C121, C122, C123, C124, C125,
 C126
 with sigma of 0.1
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. Others
 Sof(Nd1B)=Sof(O2B)=Sof(Nd2B)=Sof(Nd3B)=Sof(O3B)=Sof(O4B)=Sof(Nd4B)=Sof(Nd5B)=
 Sof(O5B)=Sof(Nd6B)=Sof(O7B)=Sof(O8B)=Sof(O9B)=Sof(O10B)=Sof(O11B)=Sof(O12B)=1-
 FVAR(1)
 Sof(Nd1A)=Sof(O2A)=Sof(Nd2A)=Sof(Nd3A)=Sof(O3A)=Sof(O4A)=Sof(Nd4A)=Sof(Nd5A)=
 Sof(O5A)=Sof(Nd6A)=Sof(O7A)=Sof(O8A)=Sof(O9A)=Sof(O10A)=Sof(O11A)=Sof(O12A)=
 FVAR(1)
5.a Fitted hexagon refined as free rotating group:
 C110(C120,C130,C140,C150,C160), C111(C112,C113,C114,C115,C116), C121(C122,
 C123,C124,C125,C126), C141(C142,C143,C144,C145,C146), C151(C152,C153,C154,C155,
 C156), C210(C220,C230,C240,C250,C260), C211(C212,C213,C214,C215,C216),
 C231(C232,C233,C234,C235,C236), C241(C242,C243,C244,C245,C246), C261(C262,C263,
 C264,C265,C266), C310(C320,C330,C340,C350,C360), C321(C322,C323,C324,C325,
 C326), C331(C332,C333,C334,C335,C336), C351(C352,C353,C354,C355,C356),
 C361(C362,C363,C364,C365,C366), C410(C420,C430,C440,C450,C460), C411(C412,C413,
 C414,C415,C416), C421(C422,C423,C424,C425,C426), C441(C442,C443,C444,C445,
 C446), C451(C452,C453,C454,C455,C456)
;
_olex2_exptl_crystal_mounting_method 'superglue on MiTeGen mount'
_olex2_submission_original_sample_id 'CJP385 Phase 2'
_olex2_submission_special_instructions 'No special instructions were received'