Quest for highly connected metal-organic framework platforms: rare-earth polynuclear clusters versatility meets net topology needs.
Alezi, Dalal; Peedikakkal, Abdul Malik P.; Weseliński, Łukasz J; Guillerm, Vincent; Belmabkhout, Youssef; Cairns, Amy J.; Chen, Zhijie; Wojtas, Łukasz; Eddaoudi, Mohamed; Journal of the American Chemical Society 137 (2015) 5421–5430; doi:10.1021/jacs.5b00450

data_4129321
_publ_section_title
;
 Quest for highly connected metal-organic framework platforms: rare-earth
 polynuclear clusters versatility meets net topology needs.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5421
_journal_page_last               5430
_journal_paper_doi               10.1021/jacs.5b00450
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C228 H108 F6 O186.5 Tb27'
_chemical_formula_weight         10235.98
_space_group_crystal_system      hexagonal
_space_group_IT_number           191
_space_group_name_Hall           '-P 6 2'
_space_group_name_H-M_alt        'P 6/m m m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.09 svn.r3130 for OlexSys, GUI svn.r4987)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   26.445(2)
_cell_length_b                   26.445(2)
_cell_length_c                   21.080(2)
_cell_measurement_reflns_used    9710
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      61.71
_cell_measurement_theta_min      3.95
_cell_volume                     12767.0(18)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD with ImuS microsource'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            53769
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        66.595
_diffrn_reflns_theta_max         66.506
_diffrn_reflns_theta_min         1.929
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.541
_exptl_absorpt_correction_T_max  0.7522
_exptl_absorpt_correction_T_min  0.5082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1320 before and 0.0622 after correction.
The Ratio of minimum to maximum transmission is 0.6756.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       plate
_exptl_crystal_F_000             4777
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.507
_refine_diff_density_min         -1.171
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4263
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1173P)^2^+88.8258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1795
_refine_ls_wR_factor_ref         0.1948
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3910
_reflns_number_total             4263
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b00450_si_002.cif
_cod_data_source_block           Tb-pek-MOF-1
_cod_original_cell_volume        12767(2)
_cod_original_formula_sum        'C228 H108 F6 O186.50 Tb27'
_cod_database_code               4129321
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.708
_shelx_estimated_absorpt_t_min   0.127
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{Tb4, O4}
3. Restrained distances
 C18-O24A
 1.26 with sigma of 0.02
 O25-O24B
 2.21 with sigma of 0.02
 C18-C16
 1.5 with sigma of 0.02
 C15-C18
 2.5 with sigma of 0.02
 C18-C17
 2.5 with sigma of 0.02
 C16-O24A
 2.37 with sigma of 0.02
 C20-O25
 2.37 with sigma of 0.02
 C20-O24B
 2.37 with sigma of 0.02
 F3-C19 = F2-C21
 1.34 with sigma of 0.02
 F3-C27 = F2-C25
 2.34 with sigma of 0.02
 F3-C20
 2.34 with sigma of 0.02
 F2-C20
 2.34 with sigma of 0.02
 C14-H14
 0.93 with sigma of 0.02
 H14-C30
 2 with sigma of 0.01
 C29-C1B = C30-C1A
 1.5 with sigma of 0.02
 C4-C3A = C4-C3B = C3A-C30 = C3B-C29 = C29-C14 = C30-C14
 1.39 with sigma of 0.01
 H14-C29_$1
 2 with sigma of 0.01
 C16-F1
 2.34 with sigma of 0.02
 F1-C22
 2.34 with sigma of 0.02
 O25-C26
 1.26 with sigma of 0.02
 O24B-C26
 1.26 with sigma of 0.02
 C26-C21
 2.5 with sigma of 0.02
 C26-C19
 2.5 with sigma of 0.02
 C18-C16 = C26-C20
 1.5 with sigma of 0.02
 O13B-C18
 1.26 with sigma of 0.02
 O24A-O13B
 2.21 with sigma of 0.02
 C16-O13B
 2.37 with sigma of 0.02
4. Restrained planarity
 C30, H14, C29_$1, C14
 with sigma of 0.1
 O24B, O25, C26, C20, C19, C27, C28, C25, C21, F2, F3
 with sigma of 0.01
 O13B, C23, C18, O24A
 with sigma of 0.001
 O13B, C16, C17, C24, C23, C22, C15, C18, F1
 with sigma of 0.01
5. Uiso/Uaniso restraints and constraints
C20 \\sim C19 \\sim C27 \\sim C28 \\sim C25 \\sim C21 \\sim F2 \\sim F3: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C16 \\sim C17 \\sim C24 \\sim C23 \\sim C22 \\sim C15 \\sim F1: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O20) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(Tb4) = Uanis(O4)
6. Others
 Fixed Sof: Tb2B(0.25) Tb3(0.125) Tb4(0.25) Tb2A(0.25) O12(0.25) O19(0.5)
 O18(0.5) O13B(0.25) O7(0.5) O8(0.125) O17(0.25) O9(0.5) C29(0.5) C3B(0.5)
 H3B(0.5) C1B(0.5) C7(0.5) H7(0.5) C10(0.5) H10(0.5) C9(0.5) H9(0.5) C6(0.5)
 H6(0.5) O4(0.25) O23(0.25) O24B(0.25) O25(0.25) C26(0.25) C16(0.125)
 C17(0.125) H17(0.125) C24(0.125) H24(0.125) C23(0.125) H23(0.125) C22(0.125)
 H22(0.125) C15(0.125) C18(0.25) C20(0.125) C19(0.125) H19(0.0625) C27(0.125)
 H27(0.125) C28(0.125) H28(0.125) C25(0.125) H25(0.125) C21(0.125) H21(0.0625)
 C1A(0.5) O24A(0.25) O26(0.0625) O2(0.02083) O5(0.125) O28(0.0625) O11(0.125)
 O13(0.0625) O16(0.25) O29(0.125) O30(0.25) F1(0.125) F2(0.0625) F3(0.0625)
 O31(0.02083) O32(0.0625) O33(0.0625) C3A(0.5) H3A(0.5) C30(0.5) O35(0.02083)
 O36(0.0625) O0(0.25)
7.a Aromatic/amide H refined with riding coordinates:
 C3B(H3B), C7(H7), C10(H10), C9(H9), C6(H6), C17(H17), C24(H24), C23(H23),
 C22(H22), C19(H19), C27(H27), C28(H28), C25(H25), C21(H21), C3A(H3A)
7.b Fitted hexagon refined as free rotating group:
 C16(C17,C24,C23,C22,C15), C20(C19,C27,C28,C25,C21)
;
_olex2_submission_special_instructions 'No special instructions were received'