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_4129322
_publ_section_title
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 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_moiety         'C240 H132 F6 O164.48 Tb27, 12(O0.38)'
_chemical_formula_sum            'C240 H132 F6 O168.5 Tb27'
_chemical_formula_weight         10116.29
_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   geom
_atom_sites_solution_primary     direct
_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                   26.3169(12)
_cell_length_b                   26.3169(12)
_cell_length_c                   26.3903(16)
_cell_measurement_reflns_used    9828
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.04
_cell_measurement_theta_min      3.35
_cell_volume                     15828.7(14)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.65
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.979
_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_R_equivalents  0.1004
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            56083
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.647
_diffrn_reflns_theta_min         3.871
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.927
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.3743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1395 before and 0.0880 after correction.
The Ratio of minimum to maximum transmission is 0.4971.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_description       plate
_exptl_crystal_F_000             4729
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.882
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         5332
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1049
_refine_ls_R_factor_gt           0.0859
_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^)+(0.1152P)^2^+187.9351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2293
_refine_ls_wR_factor_ref         0.2472
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4326
_reflns_number_total             5332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b00450_si_004.cif
_cod_data_source_block           Tb-pek-MOF-2
_cod_original_cell_volume        15828.7(17)
_cod_original_formula_sum        'C240 H132 F6 O168.50 Tb27'
_cod_database_code               4129322
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.754
_shelx_estimated_absorpt_t_min   0.229
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{Tb86, O86}
3. Restrained distances
 C78-C80
 1.5 with sigma of 0.02
 O81-C80 = O82-C80
 1.26 with sigma of 0.02
 C92-O16 = C92-O91
 1.26 with sigma of 0.02
 O16-C18
 1.26 with sigma of 0.02
 O90-C18 = O16-C18
 1.26 with sigma of 0.02
 O14-C47
 1.26 with sigma of 0.02
 F2-C93
 1.34 with sigma of 0.02
 C104-C18
 1.5 with sigma of 0.02
 C98-C92
 1.5 with sigma of 0.02
 C100-C92
 2.51 with sigma of 0.02
 C99-C92
 2.51 with sigma of 0.02
 F3-C99
 1.34 with sigma of 0.02
 C102-F3
 2.34 with sigma of 0.02
 F3-C98
 2.34 with sigma of 0.02
 C98-O91
 2.37 with sigma of 0.02
 C98-O16
 2.37 with sigma of 0.02
 O90-C104
 2.37 with sigma of 0.04
 C97-C18
 2.51 with sigma of 0.04
 C18-C93
 2.51 with sigma of 0.04
 C104-O16
 2.37 with sigma of 0.04
4. Restrained planarity
 C18, C104, C93, C94, C95, C96, C97, F2
 with sigma of 0.1
 C92, C98, C100, C101, C103, C102, C99, F3
 with sigma of 0.01
 O16, C92, C98, C100
 with sigma of 0.1
5. Rigid bond restraints
 O45, C35, O81, O82, C80, C1, C69, C76, C78, C77, C70, C56
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Uiso/Uaniso restraints and constraints
O45 \\sim O81 \\sim O82 \\sim C80 \\sim C1 \\sim C69 \\sim C76 \\sim C78 \\sim
C77 \\sim C70 \\sim C56: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C104 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim C97 \\sim F2: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
C92 \\sim C98 \\sim C100 \\sim C101 \\sim C103 \\sim C102 \\sim C99: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(Tb86) = Uanis(O86)
7. Others
 Fixed Sof: Tb86(0.25) Tb83(0.125) O15(0.25) O14(0.25) O16(0.375) O81(0.5)
 O93(0.125) O82(0.5) C80(0.5) C1(0.5) C69(0.5) H69(0.5) C76(0.5) H76(0.5)
 C78(0.5) C77(0.5) H77(0.5) C70(0.5) H70(0.5) C56(0.5) H56A(0.5) H56B(0.5)
 C18(0.125) O90(0.25) C47(0.125) O91(0.25) C104(0.125) C93(0.125) C94(0.125)
 H94(0.125) C95(0.125) H95(0.125) C96(0.125) H96(0.125) C97(0.125) H97(0.125)
 F2(0.125) C92(0.25) O94(0.25) O86(0.25) C98(0.125) C100(0.125) H100(0.125)
 C101(0.125) H101(0.125) C103(0.125) H103(0.125) C102(0.125) H102(0.125)
 C99(0.125) O96(0.125) O95(0.0625) F3(0.125)
8.a Secondary CH2 refined with riding coordinates:
 C56(H56A,H56B)
8.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C25(H25), C69(H69), C76(H76), C77(H77), C70(H70), C94(H94),
 C95(H95), C96(H96), C97(H97), C100(H100), C101(H101), C103(H103), C102(H102)
8.c Fitted hexagon refined as free rotating group:
 C1(C69,C76,C78,C77,C70), C104(C93,C94,C95,C96,C97), C98(C100,C101,C103,C102,
 C99)
;
_olex2_submission_special_instructions 'No special instructions were received'