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_4129320
_publ_section_title
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 Quest for highly connected metal-organic framework platforms: rare-earth
 polynuclear clusters versatility meets net topology needs.
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_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            'C316 H220 F4 N24 O203.27 Y30.68'
_chemical_formula_weight         10409.23
_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             2015-01-11
_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                   29.3518(16)
_cell_length_b                   29.3518(16)
_cell_length_c                   21.1634(16)
_cell_measurement_reflns_used    8931
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.29
_cell_measurement_theta_min      2.72
_cell_volume                     15790.1(17)
_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)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.985
_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  0.1034
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            92092
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.303
_diffrn_reflns_theta_min         3.011
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.167
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.6421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0948 before and 0.0680 after correction.
The Ratio of minimum to maximum transmission is 0.8527.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_description       plate
_exptl_crystal_F_000             5143
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.321
_refine_diff_density_min         -1.978
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         5394
_refine_ls_number_restraints     179
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1308
_refine_ls_R_factor_gt           0.0997
_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^)+(0.1599P)^2^+173.2457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2859
_refine_ls_wR_factor_ref         0.3214
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3909
_reflns_number_total             5394
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b00450_si_006.cif
_cod_data_source_block           Y-aea-MOF-1
_cod_original_cell_volume        15790(2)
_cod_database_code               4129320
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.593
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Y4, O5}
3. Restrained distances
 O13B-C10B = O43-C10B
 1.26 with sigma of 0.02
 N9-C27
 1.32 with sigma of 0.02
 O31-C27
 1.23 with sigma of 0.02
 N9-O31
 2.26 with sigma of 0.02
 C2B-C1B = C2A-C1A
 1.5 with sigma of 0.02
 O2-C1B = O2-C1A = O1-C1B = O1-C1A
 1.26 with sigma of 0.02
 C9B-C16B = C9A-C16A = C9A-C19A = C9B-C19B = C19A-C18A = C19B-C18B = C8B-C18B =
  C8A-C18A = C8B-C17B = C8A-C17A = C17A-C16A = C17B-C16B
 1.39 with sigma of 0.02
 C9A-C10A = C9B-C10B
 1.5 with sigma of 0.02
 O13A-C10A = O13B-C10B = O43-C10B = O43-C10A
 1.26 with sigma of 0.02
 C3A-C15A = C3B-C15B = C5A-C15A = C5B-C15B = C6B-C5B = C6A-C5A = C6A-C2A = C6B-
 C2B = C4A-C2A = C4B-C2B = C4A-C3A = C4B-C3B
 1.39 with sigma of 0.02
 C21-C20
 1.5 with sigma of 0.02
 F1-C23 = F2-C22
 1.34 with sigma of 0.02
 C74-F2
 2.34 with sigma of 0.02
 F2-C21
 2.34 with sigma of 0.02
 C21-F1
 2.34 with sigma of 0.02
 F1-C61
 2.34 with sigma of 0.02
 O30-C25
 1.23 with sigma of 0.02
 C28-C27
 2.41 with sigma of 0.02
 C57-C27
 2.41 with sigma of 0.02
 N9-C28 = N9-C57
 1.45 with sigma of 0.02
 C28-C57
 2.47 with sigma of 0.02
 N8-O30
 2.26 with sigma of 0.02
 N8-C24 = N8-C26
 1.45 with sigma of 0.02
 C26-C24
 2.47 with sigma of 0.02
 C25-N8
 1.32 with sigma of 0.02
 C25-C24
 2.41 with sigma of 0.02
 C25-C26
 2.41 with sigma of 0.02
 N7B-C8B \\sim N7A-C8A
 with sigma of 0.02
 N7B-C15B \\sim N7A-C15A
 with sigma of 0.02
4. Restrained planarity
 C20, C21, C22, C74, C98, C61, C23, F2, F1
 with sigma of 0.1
 C28, N9, C27, O31, C57
 with sigma of 0.01
5. Uiso/Uaniso restraints and constraints
O1 \\sim O2 \\sim C1B \\sim C2B \\sim C6B \\sim C4B \\sim C5B \\sim C3B \\sim
C10B \\sim C9B \\sim O43 \\sim O43 \\sim C8B \\sim N7B \\sim C15B \\sim C18B
\\sim C16B \\sim C17B \\sim C19B \\sim O13B \\sim C2A \\sim C6A \\sim C5A \\sim
C4A \\sim C3A \\sim C15A \\sim N7A \\sim C8A \\sim C17A \\sim C16A \\sim C9A
\\sim C19A \\sim C18A \\sim O13A \\sim C10A: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O33 \\sim O45 \\sim O47 \\sim O49 \\sim O50 \\sim O51 \\sim O55 \\sim O57:
within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C21 \\sim C22 \\sim C74 \\sim C98 \\sim C61 \\sim C23 \\sim F2 \\sim F1: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C28 \\sim N9 \\sim C27 \\sim O31 \\sim C57: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(O5) = Uanis(Y4)
6. Others
 Fixed Sof: C1B(0.5) C2B(0.5) C6B(0.5) H6B(0.5) C4B(0.5) H4B(0.5) C5B(0.5)
 C3B(0.5) H3B(0.5) Y3(0.125) Y4(0.25) C10B(0.25) C9B(0.25) O43(0.25)
 Y1(0.04167) Y2(0.08334) C8B(0.25) N7B(0.25) C15B(0.5) C18B(0.25) H18B(0.25)
 C16B(0.25) H16B(0.25) C17B(0.25) H17B(0.25) C19B(0.25) H19B(0.25) O13B(0.25)
 O17(0.125) O21(0.08334) O23(0.08334) O26(0.16667) O25(0.16667) O28(0.02778)
 C20(0.16667) C21(0.16667) C22(0.16667) H22(0.08333) C74(0.16667) H74(0.16667)
 C98(0.16667) H98(0.16667) C61(0.16667) H61(0.16667) C23(0.16667) H23(0.08333)
 O30(0.25) C28(0.25) H28A(0.25) H28B(0.25) H28C(0.25) O29(0.25) N9(0.25)
 N8(0.25) C24(0.25) H24A(0.25) H24B(0.25) H24C(0.25) C25(0.25) H25(0.25)
 C27(0.25) H27(0.25) C26(0.25) H26A(0.25) H26B(0.25) H26C(0.25) O31(0.25)
 F2(0.08333) F1(0.08333) C57(0.25) H57A(0.25) H57B(0.25) H57C(0.25) O32(0.125)
 O33(0.125) O35(0.125) O40(0.125) O36(0.125) O37(0.0625) C2A(0.5) C6A(0.5)
 H6A(0.5) C5A(0.5) C4A(0.5) H4A(0.5) C3A(0.5) H3A(0.5) C15A(0.5) N7A(0.25)
 C8A(0.25) C17A(0.25) H17A(0.25) C16A(0.25) H16A(0.25) C9A(0.25) C19A(0.25)
 H19A(0.25) C18A(0.25) H18A(0.25) O13A(0.25) C10A(0.25) O42(0.25) C1A(0.5)
 O44(0.08) O5(0.25) O45(0.0625) O47(0.0625) O49(0.125) O50(0.0625) O51(0.03125)
 O52(0.03125) O54(0.125) O53(0.07) O55(0.0625) O56(0.0625) O57(0.0625)
 O58(0.04167) O3A(0.25)
7.a Riding coordinates:
 C28(H28A,H28B,H28C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C57(H57A,H57B,
 H57C)
7.b Aromatic/amide H refined with riding coordinates:
 C6B(H6B), C4B(H4B), C3B(H3B), C18B(H18B), C16B(H16B), C17B(H17B), C19B(H19B),
 C22(H22), C74(H74), C98(H98), C61(H61), C23(H23), C25(H25), C27(H27), C6A(H6A),
  C4A(H4A), C3A(H3A), C17A(H17A), C16A(H16A), C19A(H19A), C18A(H18A)
7.c Fitted hexagon refined as free rotating group:
 C21(C22,C74,C98,C61,C23)
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_olex2_submission_special_instructions 'No special instructions were received'