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_1519417
_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         'C162 H78 O32 Y6'
_chemical_formula_sum            'C162 H78 O32 Y6'
_chemical_formula_weight         3069.70
_chemical_name_systematic        Y-ftw-MOF-3
_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             2015-01-29
_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                   48.111(16)
_cell_length_b                   48.111(16)
_cell_length_c                   48.111(16)
_cell_measurement_temperature    284(2)
_cell_volume                     111361(6)
_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      284(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD ImuS microfocus'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0592
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            4688
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        36.344
_diffrn_reflns_theta_max         36.344
_diffrn_reflns_theta_min         1.298
_exptl_absorpt_coefficient_mu    0.964
_exptl_absorpt_correction_T_max  0.7507
_exptl_absorpt_correction_T_min  0.4599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.366
_exptl_crystal_description       cube
_exptl_crystal_F_000             12320
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.871
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         4688
_refine_ls_number_restraints     764
_refine_ls_restrained_S_all      0.852
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0779
_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^)+(0.1747P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2006
_refine_ls_wR_factor_ref         0.2196
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2697
_reflns_number_total             4688
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc00614g2.cif
_cod_data_source_block           Y-ftw-MOF-3
_cod_depositor_comments
'Adding full bibliography for 1519415--1519417.cif.'
_cod_original_cell_volume        111362(112)
_cod_database_code               1519417
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.953
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O2BA-C5BA = O2BB-C5BB = O4AB-C5BB = O4AA-C5BA = O7B-C75 = O7A-C76 = O6BB-C75 =
  O6BB-C76
 1.26 with sigma of 0.02
 H19A-H54A
 -2.2 with sigma of 0.02
 H19B-H54B
 -2.2 with sigma of 0.02
 C8B-C5BB = C8A-C5BA = C75-C26B = C76-C26A
 1.49 with sigma of 0.02
 H42B-H57B
 -2.2 with sigma of 0.02
 C36B-C30B = C36A-C30A = C47B-C27B = C47A-C27A
 1.21 with sigma of 0.02
 C40B-C27B = C40A-C27A = C47B-C31B = C47A-C31A = C36B-C35B = C36A-C1 = C52B-
 C30B = C52A-C30A
 1.44 with sigma of 0.02
 H9-H4
 -2.2 with sigma of 0.02
 C42B_$1-C34B = C9_$1-C6 = C9-C6 = C42B-C34B = C42B-C35B = C9-C1 = C3-C1 =
 C74B-C35B = C74B-C35B_$1 = C3-C1_$1 = C9_$1-C1_$1 = C42B_$1-C35B_$1 = C57B_$1-
 C41B = C4_$1-C2 = C57B-C41B
 1.39 with sigma of 0.01
 C47B-C49B
 2.46 with sigma of 0.01
 C19B-C19B_$5
 2.38 with sigma of 0.04
 C19A-C19A_$5
 2.38 with sigma of 0.04
 C19A-C19A_$5
 2.75 with sigma of 0.04
 C19A_$2-C19A_$1
 2.75 with sigma of 0.04
 C54B-C47B
 2.46 with sigma of 0.01
 C34B-C74B
 2.79 with sigma of 0.04
 C6-C3
 2.79 with sigma of 0.04
 C35B-C42B_$1 = C42B-C35B_$1
 2.79 with sigma of 0.04
 C9-C1_$1 = C9_$1-C1
 2.79 with sigma of 0.04
3. Restrained planarity
 C22A_$1, C19A_$1, C19A, C22A, C19A_$5, C19A_$2
 with sigma of 0.1
 C2, C4_$1, C4_$4, C2_$4, C4_$3, C4
 with sigma of 0.1
 C31A_$5, C54A_$5, C29A, C54A, C31A, C49A
 with sigma of 0.1
 C19B_$2, C22B_$1, C19B_$1, C19B, C22B, C19B_$5
 with sigma of 0.1
 C29B, C54B_$5, C31B_$5, C49B, C31B, C54B
 with sigma of 0.1
 C25B, C40B, C48B, C27B
 with sigma of 0.1
 C31B, C47B, C49B, C54B
 with sigma of 0.1
 C47A, C31A, C49A, C54A
 with sigma of 0.1
 O2BB, C5BB, O4AB, C8B
 with sigma of 0.01
 C36A_$3, C30A_$3, C52A_$3, C21A_$3, C14A_$3
 with sigma of 0.1
 O2BA, C5BA, C8A, O4AA
 with sigma of 0.01
 C14B, C52B, C21B, C30B
 with sigma of 0.1
 C48A, C40A, C25A, C27A
 with sigma of 0.1
 C35B, C42B, C34B, C42B_$1, C35B_$1, C74B
 with sigma of 0.01
 C6, C9, C1, C3, C1_$1, C9_$1
 with sigma of 0.1
 C9_$3, C1_$3, C3_$4, C36A_$3, C30A_$3
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C19B \\sim C22B \\sim C26B \\sim C7B \\sim C25B \\sim C40B \\sim C48B \\sim
C10B \\sim C27B \\sim C29B \\sim C31B \\sim C47B \\sim C49B \\sim C54B \\sim
C26A \\sim C10A \\sim C48A \\sim C40A \\sim C25A \\sim C7A \\sim C27A \\sim
C47A \\sim C31A \\sim C49A \\sim C54A \\sim C29A \\sim C22A \\sim C19A \\sim
C75 \\sim O7B \\sim C76 \\sim O7A: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C8B \\sim C1B \\sim C14B \\sim C52B \\sim C21B \\sim C2B \\sim C30B \\sim C34B
\\sim C35B \\sim C36B \\sim C41B \\sim C42B \\sim C57B \\sim C74B \\sim C8A
\\sim C1A \\sim C14A \\sim C52A \\sim C21A \\sim C2A \\sim C30A \\sim C36A
\\sim C1 \\sim C3 \\sim C2 \\sim C6 \\sim C4 \\sim C9 \\sim C5BB \\sim O2BB
\\sim O4AB \\sim C5BA \\sim O4AA \\sim O2BA: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(C1A) \\sim Ueq, Uanis(C1B) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(O1) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C10A) \\sim Ueq: with sigma of 0.025 and sigma for terminal atoms of 0.05
Uanis(C9) \\sim Ueq: with sigma of 0.025 and sigma for terminal atoms of 0.05
5. Others
 Sof(C19B)=Sof(H19B)=Sof(C26B)=Sof(C7B)=Sof(H7B)=Sof(C25B)=Sof(H25B)=Sof(C40B)=
 Sof(C48B)=Sof(H48B)=Sof(C10B)=Sof(H10B)=Sof(C27B)=Sof(C31B)=Sof(C47B)=
 Sof(C54B)=Sof(H54B)=Sof(C75)=Sof(O7B)=1-FVAR(1)
 Sof(C22B)=Sof(C29B)=Sof(C49B)=Sof(H49B)=0.5*(1-FVAR(2))
 Sof(C49A)=Sof(H49A)=Sof(C29A)=Sof(C22A)=0.5*FVAR(2)
 Sof(C26A)=Sof(C10A)=Sof(H10A)=Sof(C48A)=Sof(H48A)=Sof(C40A)=Sof(C25A)=
 Sof(H25A)=Sof(C7A)=Sof(H7A)=Sof(C27A)=Sof(C47A)=Sof(C31A)=Sof(C54A)=Sof(H54A)=
 Sof(C19A)=Sof(H19A)=Sof(C76)=Sof(O7A)=FVAR(1)
 Sof(C8B)=Sof(C1B)=Sof(H1B)=Sof(C14B)=Sof(H14B)=Sof(C52B)=Sof(C21B)=Sof(H21B)=
 Sof(C2B)=Sof(H2B)=Sof(C30B)=Sof(C35B)=Sof(C36B)=Sof(C42B)=Sof(H42B)=Sof(C57B)=
 Sof(H57B)=Sof(C5BB)=Sof(O2BB)=Sof(O4AB)=1-FVAR(2)
 Sof(C34B)=Sof(C41B)=Sof(C74B)=Sof(H74B)=0.5*(1-FVAR(3))
 Sof(C3)=Sof(H3)=Sof(C2)=Sof(C6)=0.5*FVAR(3)
 Sof(C8A)=Sof(C1A)=Sof(H1A)=Sof(C14A)=Sof(H14A)=Sof(C52A)=Sof(C21A)=Sof(H21A)=
 Sof(C2A)=Sof(H2A)=Sof(C30A)=Sof(C36A)=Sof(C1)=Sof(C4)=Sof(H4)=Sof(C9)=Sof(H9)=
 Sof(C5BA)=Sof(O4AA)=Sof(O2BA)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C1B(H1B), C14B(H14B), C21B(H21B), C2B(H2B), C19B(H19B), C7B(H7B), C25B(H25B),
 C48B(H48B), C10B(H10B), C42B(H42B), C49B(H49B), C54B(H54B), C57B(H57B),
 C74B(H74B), C1A(H1A), C14A(H14A), C21A(H21A), C2A(H2A), C3(H3), C4(H4), C9(H9),
  C10A(H10A), C48A(H48A), C25A(H25A), C7A(H7A), C49A(H49A), C54A(H54A),
 C19A(H19A)
6.b Fitted hexagon refined as free rotating group:
 C8B(C1B,C14B,C52B,C21B,C2B), C26B(C7B,C25B,C40B,C48B,C10B), C8A(C1A,C14A,C52A,
 C21A,C2A), C26A(C10A,C48A,C40A,C25A,C7A)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'