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_4129319
_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            'C261 H195 F6 N12 O168 Y27'
_chemical_formula_weight         8701.85
_space_group_crystal_system      hexagonal
_space_group_IT_number           193
_space_group_name_Hall           '-P 6c 2'
_space_group_name_H-M_alt        'P 63/m c m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-12-23
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   25.9989(15)
_cell_length_b                   25.9989(15)
_cell_length_c                   42.656(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.594
_cell_measurement_theta_min      26.951
_cell_volume                     24970(3)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.65
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD with ImuS Cu microsource'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            97625
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        66.595
_diffrn_reflns_theta_max         67.496
_diffrn_reflns_theta_min         4.441
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.596
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.5835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0921 before and 0.0481 after correction.
The Ratio of minimum to maximum transmission is 0.7750.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_description       plate
_exptl_crystal_F_000             8592
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.027
_refine_diff_density_min         -1.825
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         7856
_refine_ls_number_restraints     173
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0730
_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^)+(0.0978P)^2^+265.2155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2067
_refine_ls_wR_factor_ref         0.2170
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7025
_reflns_number_total             7856
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b00450_si_003.cif
_cod_data_source_block           Y-pek-MOF-1
_cod_database_code               4129319
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.445
_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
{Y5, O13}
3. Restrained distances
 O43-C15
 1.23 with sigma of 0.02
 O42-C83 = O7-C83
 1.26 with sigma of 0.02
 N2-C81
 1.32 with sigma of 0.02
 O28-C81
 1.23 with sigma of 0.02
 N2-O28
 2.26 with sigma of 0.02
 O47-C85 = O48-C85
 1.26 with sigma of 0.02
 C89-C29 = C89-C88 = C88-C41 = C86-C41 = C87-C86 = C87-C29
 1.39 with sigma of 0.02
 F8-C90
 1.34 with sigma of 0.02
 N2-O28
 2.26 with sigma of 0.02
 O47-O48
 2.21 with sigma of 0.02
 O8-C9 = O7-C9 = O26B-C2 = O18-C2
 1.26 with sigma of 0.02
 N1-C91
 1.32 with sigma of 0.02
 O17-C91
 1.23 with sigma of 0.02
 N1-O17
 2.26 with sigma of 0.02
 N2-C82
 1.45 with sigma of 0.02
 N2-C84
 1.45 with sigma of 0.02
 C82-C84
 2.47 with sigma of 0.02
 C84-C81
 2.41 with sigma of 0.02
 C81-C82
 2.41 with sigma of 0.02
 C82-C81
 2.41 with sigma of 0.02
 C1-C6
 2.47 with sigma of 0.02
 C15-C6
 2.41 with sigma of 0.02
 C1-C15
 2.41 with sigma of 0.02
 N1-C17 = N1-C8
 1.45 with sigma of 0.02
 C17-C8
 2.47 with sigma of 0.02
 C17-C91
 2.41 with sigma of 0.02
 C8-C91
 2.41 with sigma of 0.02
 C15-N35
 1.32 with sigma of 0.02
 O43-N35
 2.26 with sigma of 0.02
 N35-C1
 1.45 with sigma of 0.02
 N35-C6
 1.45 with sigma of 0.02
4. Restrained planarity
 C2, C5, C7, C3, C2AA, C4, C25, F9
 with sigma of 0.01
 C29, C89, C88, C41, C86, C87
 with sigma of 0.01
 C80, C14, C10, C12, C26, C90, F8
 with sigma of 0.01
 C9, C80, C14, C10, C12, C26, C90, F8
 with sigma of 0.01
 O28, N2, C81, C82
 with sigma of 0.1
 O28, N2, C81, C82, C84
 with sigma of 0.1
 O43, C15, N35, C1, C6
 with sigma of 0.01
5. Rigid bond restraints
 C83, O42
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Uiso/Uaniso restraints and constraints
C2 \\sim C5 \\sim C7 \\sim C3 \\sim C2AA \\sim C4 \\sim C25: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
O26B \\sim C2 \\sim O10 \\sim O27 \\sim O18: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O46 \\sim C85: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
O48 \\sim O46 \\sim O47 \\sim O15A \\sim C85: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
Y49 \\sim O14: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
O8 \\sim O8: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
O8 \\sim O45: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N2 \\sim C84: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
O42 \\sim C83: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(Y5) = Uanis(O13)
Uanis(O14) = Uanis(Y49)
7. Others
 Fixed Sof: O26B(0.25) C47(0.85) H47(0.85) C51(0.85) H51(0.85) C55(0.85)
 H55(0.85) Y4(0.2125) Y5(0.425) C78(0.85) H78(0.85) Y6(0.0375) O1(0.2125)
 C9(0.25) C80(0.25) C14(0.25) H14(0.25) C10(0.25) H10(0.25) C12(0.25) H12(0.25)
 C26(0.25) H26(0.25) C90(0.25) C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5) O17(0.5)
 C91(0.5) H91(0.5) C2(0.25) N1(0.5) C5(0.25) C7(0.25) C3(0.25) H3(0.25)
 C2AA(0.25) H2AA(0.25) C4(0.25) H4(0.25) C25(0.25) H25(0.25) C8(0.5) H8A(0.5)
 H8B(0.5) H8C(0.5) O10(0.25) O27(0.25) O8(0.25) O28(0.16667) N2(0.16667)
 O34(0.2125) O36(0.0375) N35(0.33333) O18(0.25) O42(0.25) F9(0.25) F8(0.25)
 C81(0.16667) H81(0.16667) C82(0.16667) H82A(0.16667) H82B(0.16667)
 H82C(0.16667) O43(0.33333) C1(0.33333) H1A(0.33333) H1B(0.33333) H1C(0.33333)
 C6(0.33333) H6A(0.33333) H6B(0.33333) H6C(0.33333) C15(0.33333) H15(0.33333)
 O45(0.25) C83(0.25) H83(0.25) C84(0.16667) H84A(0.16667) H84B(0.16667)
 H84C(0.16667) O15A(0.85) O46(0.85) O47(0.15) O48(0.15) O14(0.425) Y49(0.075)
 C86(0.15) H86(0.15) C88(0.15) H88(0.15) C87(0.15) H87(0.15) C89(0.15)
 H89(0.15) O44A(0.25) O49(0.125) O50(0.02083) O51(0.0625) O54(0.0625)
 O52(0.0625) O53(0.125) O56(0.0625) O55(0.0625) O57(0.2125) O13(0.075)
8.a Riding coordinates:
 C83(H83)
8.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C18(H18), C20(H20), C47(H47), C51(H51), C55(H55), C78(H78),
 C14(H14), C10(H10), C12(H12), C26(H26), C91(H91), C3(H3), C2AA(H2AA), C4(H4),
 C25(H25), C81(H81), C15(H15), C86(H86), C88(H88), C87(H87), C89(H89)
8.c Fitted hexagon refined as free rotating group:
 C80(C14,C10,C12,C26,C90), C5(C7,C3,C2AA,C4,C25)
8.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C8(H8A,H8B,H8C), C82(H82A,H82B,H82C), C1(H1A,H1B,H1C),
 C6(H6A,H6B,H6C), C84(H84A,H84B,H84C)
;
_olex2_submission_special_instructions 'No special instructions were received'