All Roads Lead to Rome: Tuning the Luminescence of a Breathing Catenated Zr-MOF by Programmable Multiplexing Pathways
Chen, Cheng-Xia; Wei, Zhang-Wen; Cao, Chen-Chen; Yin, Shao-Yun; Qiu, Qian-Feng; Zhu, Neng-Xiu; Xiong, Yang-Yang; Jiang, Ji-Jun; Pan, Mei; Su, Cheng-Yong; Chemistry of Materials 31 (2019) 5550–; doi:10.1021/acs.chemmater.9b01258

data_4003038
_publ_section_title
;
 All Roads Lead to Rome: Tuning the Luminescence of a Breathing Catenated
 Zr-MOF by Programmable Multiplexing Pathways
;
_journal_issue                   15
_journal_name_full               'Chemistry of Materials'
_journal_page_first              5550
_journal_paper_doi               10.1021/acs.chemmater.9b01258
_journal_volume                  31
_journal_year                    2019
_chemical_formula_moiety         'C108 H64 O32 Zr6 [+ solvent]'
_chemical_formula_sum            'C108 H64 O32 Zr6'
_chemical_formula_weight         2420.91
_chemical_name_common            LIFM-114-Toluene
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-12-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.6952(15)
_cell_length_b                   41.2943(11)
_cell_length_c                   16.8339(6)
_cell_measurement_reflns_used    7581
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      65.2550
_cell_measurement_theta_min      4.4440
_cell_volume                     18557.0(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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    -75.00  39.00   1.00   70.00    --  -41.14  19.00  60.00  114
  2  \w      4.00  31.00   1.00   70.00    --   41.14 -99.00 -90.00   27
  3  \w     78.00 160.00   1.00   72.00    --   89.96  61.00-180.00   82
  4  \w    102.00 138.00   1.00   72.00    --   89.96 125.00  30.00   36
  5  \w    124.00 158.00   1.00   72.00    --   89.96 125.00-180.00   34
  6  \w     97.00 160.00   1.00   72.00    --   89.96 125.00  90.00   63
  7  \w     72.00 109.00   1.00   72.00    --   89.96  30.00-180.00   37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0475539000
_diffrn_orient_matrix_UB_12      -0.0202901000
_diffrn_orient_matrix_UB_13      0.0144380000
_diffrn_orient_matrix_UB_21      0.0061350000
_diffrn_orient_matrix_UB_22      -0.0157258000
_diffrn_orient_matrix_UB_23      -0.0824224000
_diffrn_orient_matrix_UB_31      0.0320752000
_diffrn_orient_matrix_UB_32      -0.0270795000
_diffrn_orient_matrix_UB_33      0.0371522000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            22133
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        65.362
_diffrn_reflns_theta_max         65.362
_diffrn_reflns_theta_min         3.283
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.045
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    0.867
_exptl_crystal_description       Rod
_exptl_crystal_F_000             4832
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
TITL exp_2229 in Cmcm
CELL   26.6952   41.2943   16.8339     90.00     90.00     90.00
SPGR Cmcm
Q101 0.329 0.242 0.243 !       3.20 eA-3
C102 0.500 0.078 0.247 !       2.70 eA-3
C103 0.689 0.148 0.247 !       2.35 eA-3
C104 0.734 0.156 0.259 !       2.28 eA-3
C105 0.659 0.313 0.249 !       2.27 eA-3
C106 0.485 0.406 0.250 !       2.18 eA-3
C107 0.828 0.156 0.254 !       1.85 eA-3
C108 0.679 0.336 0.253 !       1.85 eA-3
C109 1.000 0.484 0.254 !       1.76 eA-3
C110 0.500 0.031 0.251 !       1.63 eA-3
C111 1.000 0.330 0.013 !       1.60 eA-3
Q112 0.500 0.133 0.250 !       1.47 eA-3
C113 0.597 0.461 0.249 !       1.38 eA-3
C114 0.500 0.014 0.147 !       1.36 eA-3
Q115 0.086 0.268 0.110 !       1.36 eA-3
C116 0.977 0.160 0.340 !       1.35 eA-3
C117 1.000 0.324 0.160 !       1.35 eA-3
C118 0.742 0.176 0.209 !       1.30 eA-3
C119 0.500 0.417 0.467 !       1.29 eA-3
C120 0.614 0.445 0.251 !       1.27 eA-3
C121 0.704 0.244 0.477 !       1.26 eA-3
C122 0.828 0.352 0.248 !       1.26 eA-3
C123 1.000 0.321 0.222 !       1.25 eA-3
C124 0.795 0.203 0.172 !       1.25 eA-3
C125 0.909 0.383 0.251 !       1.25 eA-3
C126 1.000 0.141 0.380 !       1.23 eA-3
C127 0.219 0.352 0.249 !       1.23 eA-3
C128 0.532 0.039 0.266 !       1.23 eA-3
C129 0.585 0.465 0.312 !       1.22 eA-3
C130 0.431 0.430 0.255 !       1.22 eA-3
C131 1.000 0.198 0.476 !       1.20 eA-3
C132 1.000 0.171 0.115 !       1.19 eA-3
C133 0.423 0.414 0.248 !       1.19 eA-3
C134 0.381 0.063 0.250 !       1.18 eA-3
C135 0.298 0.375 0.246 !       1.16 eA-3
C136 0.953 0.148 0.244 !       1.15 eA-3
C137 0.464 0.022 0.291 !       1.15 eA-3
C138 0.446 0.461 0.255 !       1.15 eA-3
Q139 0.477 0.336 0.245 !       1.14 eA-3
C140 0.036 0.476 0.803 !       1.14 eA-3
C141 0.702 0.328 0.254 !       1.13 eA-3
C142 1.000 0.134 0.321 !       1.12 eA-3
C143 0.969 0.114 0.180 !       1.12 eA-3
C144 0.843 0.180 0.284 !       1.11 eA-3
C145 0.780 0.289 0.073 !       1.11 eA-3
C146 1.000 0.376 0.375 !       1.09 eA-3
C147 0.685 0.322 0.215 !       1.07 eA-3
C148 0.822 0.312 0.249 !       1.07 eA-3
C149 0.446 0.031 0.186 !       1.06 eA-3
C150 1.000 0.222 0.060 !       1.06 eA-3
C151 0.569 0.031 0.250 !       1.06 eA-3
C152 0.960 0.137 0.151 !       1.06 eA-3
Q153 0.969 0.211 0.483 !       1.05 eA-3
C154 0.500 0.102 0.243 !       1.05 eA-3
C155 0.459 0.016 0.254 !       1.04 eA-3
C156 0.507 0.008 0.248 !       1.03 eA-3
Q157 0.929 0.246 0.460 !       1.03 eA-3
C158 0.737 0.352 0.253 !       1.03 eA-3
C159 1.000 0.071 0.449 !       1.02 eA-3
C160 0.875 0.344 0.254 !       1.01 eA-3
C161 0.750 0.370 0.217 !       1.00 eA-3
C162 0.211 0.145 0.282 !       1.00 eA-3
C163 1.000 0.353 0.051 !       1.00 eA-3
C164 0.289 0.349 0.780 !       1.00 eA-3
C165 0.975 0.078 0.241 !       1.00 eA-3
C166 0.562 0.022 0.330 !       0.99 eA-3
C167 0.622 0.451 0.214 !       0.98 eA-3
Q168 0.288 0.242 0.254 !       0.98 eA-3
C169 0.447 0.045 0.294 !       0.98 eA-3
C170 0.476 0.463 0.127 !       0.98 eA-3
C171 0.027 0.469 0.836 !       0.98 eA-3
C172 1.000 0.461 0.015 !       0.98 eA-3
Q173 1.000 0.255 0.484 !       0.97 eA-3
C174 0.969 0.023 0.250 !       0.97 eA-3
C175 1.000 0.468 0.153 !       0.97 eA-3
C176 0.462 0.485 0.393 !       0.96 eA-3
C177 0.025 0.068 0.507 !       0.96 eA-3
C178 0.539 0.459 0.311 !       0.96 eA-3
C179 1.000 0.110 0.180 !       0.96 eA-3
C180 0.038 0.312 0.253 !       0.96 eA-3
C181 0.438 0.366 0.803 !       0.96 eA-3
C182 0.062 0.134 0.197 !       0.96 eA-3
C183 0.857 0.164 0.251 !       0.95 eA-3
C184 0.034 0.319 0.201 !       0.95 eA-3
C185 0.500 0.478 0.393 !       0.95 eA-3
C186 0.906 0.141 0.248 !       0.95 eA-3
C187 0.362 0.453 0.253 !       0.94 eA-3
C188 0.372 0.440 0.186 !       0.94 eA-3
C189 0.048 0.383 0.251 !       0.94 eA-3
C190 0.312 0.117 0.249 !       0.93 eA-3
C191 0.877 0.383 0.244 !       0.93 eA-3
C192 0.099 0.402 0.215 !       0.92 eA-3
C193 0.040 0.148 0.178 !       0.92 eA-3
C194 0.396 0.471 0.159 !       0.92 eA-3
C195 0.486 0.015 0.422 !       0.92 eA-3
C196 0.500 0.448 0.343 !       0.92 eA-3
Q197 0.952 0.285 0.042 !       0.91 eA-3
C198 0.979 0.170 0.215 !       0.91 eA-3
C199 0.261 0.383 0.246 !       0.91 eA-3
;
_refine_diff_density_max         2.537
_refine_diff_density_min         -1.900
_refine_diff_density_rms         0.126
_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     411
_refine_ls_number_reflns         8263
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0808
_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^)+(0.1344P)^2^+149.8417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2438
_refine_ls_wR_factor_ref         0.2535
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6126
_reflns_number_total             8263
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            LIFM-114-Toluene-solved.cif
_cod_data_source_block           LIFM-114-Toluene
_cod_database_code               4003038
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 C2, C3, C4, C5, C6, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C9(0.5) H9(0.5) C10(0.5) H10(0.5) C12(0.5) H12(0.5) C13(0.5)
 H13(0.5) C16(0.5) H16(0.5) C17(0.5) H17(0.5) C19(0.5) H19(0.5) C20(0.5)
 H20(0.5) C9A(0.5) H9A(0.5) C10A(0.5) H10A(0.5) C12A(0.5) H12A(0.5) C13A(0.5)
 H13A(0.5) C16A(0.5) H16A(0.5) C17A(0.5) H17A(0.5) C19A(0.5) H19A(0.5)
 C20A(0.5) H20A(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13),
 C16(H16), C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C25(H25), C26(H26),
  C9A(H9A), C10A(H10A), C12A(H12A), C13A(H13A), C16A(H16A), C17A(H17A),
 C19A(H19A), C20A(H20A)
;
_platon_squeeze_void_probe_radius 1.20
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.569
_oxdiff_exptl_absorpt_empirical_full_min 0.501