Versatile rare earth hexanuclear clusters for the design and synthesis of highly-connectedftw-MOFs
Luebke, Ryan; Belmabkhout, Youssef; Weseliński, Łukasz J.; Cairns, Amy J.; Alkordi, Mohamed; Norton, George; Wojtas, Łukasz; Adil, Karim; Eddaoudi, Mohamed; Chem. Sci. 6 (2015) 4095–; doi:10.1039/C5SC00614G

data_1519416
_publ_section_title
;
 Versatile rare earth hexanuclear clusters for the design and synthesis of
 highly-connectedftw-MOFs
;
_journal_issue                   7
_journal_name_full               'Chem. Sci.'
_journal_page_first              4095
_journal_paper_doi               10.1039/C5SC00614G
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         '0.13(C1104 H624 O280 Y48)'
_chemical_formula_sum            'C138 H78 O35 Y6'
_chemical_formula_weight         2829.46
_chemical_name_systematic        Y-ftw-MOF-2
_space_group_crystal_system      cubic
_space_group_IT_number           204
_space_group_name_Hall           '-I 2 2 3'
_space_group_name_H-M_alt        'I m -3'
_symmetry_space_group_name_Hall  '-I 2 2 3'
_symmetry_space_group_name_H-M   'I m -3'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-02-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-02-17 deposited with the CCDC.
2015-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   40.048(3)
_cell_length_b                   40.048(3)
_cell_length_c                   40.048(3)
_cell_measurement_reflns_used    3354
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      45.23
_cell_measurement_theta_min      3.12
_cell_volume                     64231(8)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD ImuS microfocus'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0803
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            4464
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        44.461
_diffrn_reflns_theta_max         44.461
_diffrn_reflns_theta_min         3.823
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.655
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.4843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0989 before and 0.0822 after correction.
The Ratio of minimum to maximum transmission is 0.6457.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.585
_exptl_crystal_description       cube
_exptl_crystal_F_000             11360
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
;
_refine_diff_density_max         2.272
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4464
_refine_ls_number_restraints     346
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.1233
_refine_ls_R_factor_gt           0.0983
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1350P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2380
_refine_ls_wR_factor_ref         0.2493
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2605
_reflns_number_total             4464
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc00614g2.cif
_cod_data_source_block           Y-ftw-MOF-2
_cod_depositor_comments
'Adding full bibliography for 1519415--1519417.cif.'
_cod_original_cell_volume        64229(13)
_cod_database_code               1519416
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.984
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O1-C24 = O2-C24
 1.25 with sigma of 0.02
 C13-C13_$6 = C5-C5_$4
 2.8 with sigma of 0.02
 C58-C5 = C8-C5 = C18-C13 = C7-C13
 1.39 with sigma of 0.01
 C58-C8
 2.39 with sigma of 0.02
 C58-C8_$7
 2.8 with sigma of 0.02
 C18-C7
 2.39 with sigma of 0.02
 C18-C7_$5
 2.8 with sigma of 0.02
 C58-C58_$7 = C18-C18_$5 = C8-C8_$7 = C7-C7_$5
 1.39 with sigma of 0.01
 C6-C1 = C32-C6 = C46-C32
 1.39 with sigma of 0.01
 C16-C15 = C19-C15 = C19-C14
 1.39 with sigma of 0.01
 H22-H16
 -2.2 with sigma of 0.02
 C9-C25 = C6-C2 = C14-C13 = C5-C46 = C20-C15
 1.49 with sigma of 0.02
 C24-C23 = C9-C25
 1.49 with sigma of 0.005
 C6_$1-C32 = C6-C32_$1 = C1_$1-C46_$1
 2.8 with sigma of 0.04
 C24-C21 = C24-C27
 2.5 with sigma of 0.04
 C6_$2-C6_$3 = C32_$3-C32_$2
 2.41 with sigma of 0.04
 C15-C19_$1 = C15_$1-C19 = C16-C14
 2.8 with sigma of 0.04
 C11-C25 = C60-C25
 2.5 with sigma of 0.04
3. Restrained planarity
 C23, C21, C22, C20, C28, C27
 with sigma of 0.1
 C32, C46_$1, C32_$1, C5_$1
 with sigma of 0.1
 C13, C7, C7_$5, C13_$6, C18_$5, C18
 with sigma of 0.1
 C5, C8, C8_$7, C5_$4, C58_$7, C58
 with sigma of 0.1
 C16, C15, C19, C14, C19_$1, C15_$1
 with sigma of 0.1
 C13, C14, C19_$1, C19, C15_$1, C15, C16
 with sigma of 0.1
 C6, C32, C46, C32_$1, C6_$1, C1, C2
 with sigma of 0.1
 C25, C9, C11, C3, C2, C4, C60, C6
 with sigma of 0.1
4. Rigid bond restraints
 C13, C14, C15, C16, C19, C23, C21, C22, C20, C28, C27, C24, O1, O2, C18, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, C3, C4, C9, C11, C25, C60, O4, O5, C1, C6, C32, C46, C5, C58, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C13 \\sim C14 \\sim C15 \\sim C16 \\sim C19 \\sim C23 \\sim C21 \\sim C22 \\sim
C20 \\sim C28 \\sim C27 \\sim C24 \\sim O1 \\sim O2 \\sim C18 \\sim C7: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C2 \\sim C3 \\sim C4 \\sim C9 \\sim C11 \\sim C25 \\sim C60 \\sim O4 \\sim O5
\\sim C1 \\sim C6 \\sim C32 \\sim C46 \\sim C5 \\sim C58 \\sim C8: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O3) \\sim Ueq: with sigma of 0.00625 and sigma for terminal atoms of
0.0125
Uanis(C25) \\sim Ueq: with sigma of 0.025 and sigma for terminal atoms of 0.05
6. Others
 Fixed Sof: C13(0.5) C18(0.5) H18(0.5) C58(0.5) H58(0.5) C7(0.5) H7(0.5)
 C8(0.5) H8(0.5) O7(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C3(H3), C4(H4), C60(H60), C16(H16), C19(H19), C21(H21), C22(H22),
 C28(H28), C27(H27), C1(H1), C32(H32), C18(H18), C58(H58), C7(H7), C8(H8)
7.b Fitted hexagon refined as free rotating group:
 C9(C11,C3,C2,C4,C60), C23(C21,C22,C20,C28,C27)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'