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_4003032
_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-Ethanol
_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                   24.4853(11)
_cell_length_b                   42.1654(14)
_cell_length_c                   17.1403(6)
_cell_measurement_reflns_used    6415
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      63.1830
_cell_measurement_theta_min      4.4370
_cell_volume                     17696.2(12)
_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 0.975
_diffrn_measured_fraction_theta_max 0.975
_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   -110.00 -16.00   1.00   15.00    --  -40.77 -38.00 -60.00   94
  2  \w     62.00 128.00   1.00   15.00    --   40.77-178.00-180.00   66
  3  \w     66.00 158.00   1.00   60.00    --   86.42  77.00-120.00   92
  4  \w     15.00 118.00   1.00   60.00    --   86.42 -77.00 150.00  103
  5  \w     94.00 157.00   1.00   60.00    --   86.42 125.00-180.00   63
  6  \w     23.00  90.00   1.00   60.00    --   86.42-125.00  60.00   67
;
_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      0.0276925000
_diffrn_orient_matrix_UB_12      0.0328421000
_diffrn_orient_matrix_UB_13      0.0003161000
_diffrn_orient_matrix_UB_21      -0.0416914000
_diffrn_orient_matrix_UB_22      0.0119935000
_diffrn_orient_matrix_UB_23      -0.0603864000
_diffrn_orient_matrix_UB_31      -0.0380995000
_diffrn_orient_matrix_UB_32      0.0107200000
_diffrn_orient_matrix_UB_33      0.0665168000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26316
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        63.567
_diffrn_reflns_theta_max         63.567
_diffrn_reflns_theta_min         3.317
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.193
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63770
_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    0.909
_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 1 in Cmcm
CELL   24.4853   42.1654   17.1403     90.00     90.00     90.00
SPGR Cmcm
C101 1.000 0.187 0.029 !       3.41 eA-3
C102 1.000 0.313 0.433 !       2.39 eA-3
C103 0.313 0.141 0.251 !       2.14 eA-3
C104 0.304 0.320 0.243 !       2.11 eA-3
C105 0.307 0.203 0.247 !       2.05 eA-3
C106 1.000 0.342 0.397 !       1.98 eA-3
C107 0.290 0.359 0.252 !       1.92 eA-3
C108 0.955 0.291 0.076 !       1.91 eA-3
C109 1.000 0.296 0.036 !       1.90 eA-3
C110 0.500 0.034 0.005 !       1.65 eA-3
C111 0.412 0.055 0.263 !       1.36 eA-3
Q112 0.500 0.198 0.460 !       1.36 eA-3
C113 0.022 0.173 0.415 !       1.35 eA-3
Q114 0.649 0.195 0.252 !       1.31 eA-3
C115 0.572 0.437 0.254 !       1.31 eA-3
C116 1.000 0.467 0.145 !       1.31 eA-3
C117 1.000 0.141 0.406 !       1.30 eA-3
C118 0.553 0.016 0.250 !       1.29 eA-3
C119 0.721 0.303 0.209 !       1.27 eA-3
Q120 0.275 0.304 0.324 !       1.26 eA-3
C121 0.390 0.453 0.231 !       1.21 eA-3
C122 0.008 0.013-0.003 !       1.19 eA-3
C123 0.500 0.478 0.446 !       1.17 eA-3
C124 0.875 0.359 0.248 !       1.16 eA-3
C125 0.271 0.211 0.098 !       1.16 eA-3
C126 0.229 0.289 0.902 !       1.16 eA-3
C127 0.548 0.414 0.235 !       1.15 eA-3
C128 1.000 0.155 0.441 !       1.14 eA-3
Q129 0.914 0.221 0.412 !       1.13 eA-3
Q130 0.900 0.241 0.034 !       1.13 eA-3
Q131 0.571 0.313 0.139 !       1.11 eA-3
C132 0.939 0.201 0.096 !       1.09 eA-3
C133 1.000 0.477 0.258 !       1.07 eA-3
C134 1.000 0.329 0.155 !       1.02 eA-3
C135 0.547 0.484 0.247 !       1.01 eA-3
C136 1.000 0.078 0.034 !       1.01 eA-3
C137 0.117 0.133 0.243 !       1.01 eA-3
C138 0.716 0.336 0.209 !       1.00 eA-3
Q139 0.500 0.315 0.450 !       1.00 eA-3
Q140 0.508 0.164 0.222 !       0.98 eA-3
C141 1.000 0.450 0.153 !       0.97 eA-3
C142 0.158 0.309 0.181 !       0.97 eA-3
Q143 0.257 0.287 0.095 !       0.97 eA-3
C144 1.000 0.039 0.308 !       0.97 eA-3
Q145 0.646 0.312 0.256 !       0.96 eA-3
Q146 0.500 0.227 0.244 !       0.95 eA-3
C147 1.000 0.023 0.248 !       0.95 eA-3
C148 0.462 0.493 0.204 !       0.95 eA-3
C149 1.000 0.066 0.420 !       0.94 eA-3
C150 0.484 0.505 0.443 !       0.94 eA-3
C151 0.484 0.496 0.036 !       0.94 eA-3
C152 0.428 0.452 0.305 !       0.94 eA-3
C153 0.757 0.203 0.384 !       0.93 eA-3
Q154 0.258 0.221 0.330 !       0.93 eA-3
Q155 0.500 0.336 0.258 !       0.93 eA-3
C156 0.130 0.317 0.276 !       0.92 eA-3
C157 1.000 0.039 0.016 !       0.92 eA-3
C158 0.423 0.414 0.272 !       0.92 eA-3
C159 0.741 0.234 0.247 !       0.92 eA-3
C160 1.000 0.464 0.217 !       0.91 eA-3
C161 1.000 0.458 0.310 !       0.91 eA-3
C162 0.630 0.176 0.786 !       0.91 eA-3
C163 1.000 0.449 0.048 !       0.90 eA-3
C164 0.896 0.149 0.248 !       0.90 eA-3
C165 0.711 0.170 0.194 !       0.90 eA-3
C166 0.423 0.465 0.290 !       0.90 eA-3
C167 0.969 0.487 0.283 !       0.90 eA-3
C168 1.000 0.041 0.399 !       0.90 eA-3
Q169 0.500 0.367 0.248 !       0.88 eA-3
C170 1.000 0.006 0.203 !       0.87 eA-3
C171 0.437 0.044 0.309 !       0.87 eA-3
C172 1.000 0.430 0.154 !       0.87 eA-3
C173 1.000 0.492 0.292 !       0.87 eA-3
C174 0.500 0.492 0.254 !       0.87 eA-3
C175 0.718 0.206 0.207 !       0.86 eA-3
C176 1.000 0.150 0.343 !       0.85 eA-3
C177 1.000 0.147 0.187 !       0.85 eA-3
C178 1.000 0.060 0.165 !       0.85 eA-3
C179 1.000 0.006 0.411 !       0.85 eA-3
C180 0.955 0.157 0.381 !       0.83 eA-3
C181 1.000 0.430 0.240 !       0.83 eA-3
C182 0.126 0.660 0.783 !       0.83 eA-3
C183 0.961 0.008 0.249 !       0.83 eA-3
C184 0.476 0.436 0.318 !       0.83 eA-3
C185 0.564 0.039 0.245 !       0.83 eA-3
C186 1.000 0.049 0.457 !       0.82 eA-3
C187 1.000 0.445 0.262 !       0.82 eA-3
C188 0.133 0.181 0.284 !       0.82 eA-3
C189 1.000 0.051 0.144 !       0.81 eA-3
C190 0.764 0.210 0.080 !       0.80 eA-3
Q191 0.107 0.237 0.108 !       0.80 eA-3
C192 0.164 0.192 0.316 !       0.79 eA-3
Q193 1.000 0.233 0.057 !       0.79 eA-3
Q194 0.025 0.266 0.451 !       0.79 eA-3
C195 0.831 0.217 0.195 !       0.79 eA-3
C196 0.500 0.445 0.144 !       0.79 eA-3
C197 0.086 0.272 0.388 !       0.79 eA-3
Q198 0.697 0.233 0.333 !       0.78 eA-3
C199 1.000 0.172 0.244 !       0.78 eA-3
;
_refine_diff_density_max         1.716
_refine_diff_density_min         -1.550
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         7543
_refine_ls_number_restraints     172
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0706
_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^)+(0.1034P)^2^+143.6003P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1983
_refine_ls_wR_factor_ref         0.2197
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5200
_reflns_number_total             7543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            LIFM-114-Ethanol-solved.cif
_cod_data_source_block           LIFM-114-Ethanol
_cod_database_code               4003032
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     59.94
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O3-O3_$1
 3.2 with sigma of 0.01
3. Rigid bond restraints
 O3, O4, C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C15, C16, C17, C18, C19, C20, C16A, C17A, C19A, C20A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O3 \\sim O4 \\sim C27: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C16A \\sim C17A
\\sim C19A \\sim C20A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C27) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. 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)
6.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 1.578
_oxdiff_exptl_absorpt_empirical_full_min 0.767