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_4129323
_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            'C270 H209 F6 N11 O187.5 Y27'
_chemical_formula_weight         9122.04
_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                   26.1763(9)
_cell_length_b                   26.1763(9)
_cell_length_c                   26.3956(11)
_cell_measurement_reflns_used    9836
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.59
_cell_measurement_theta_min      3.77
_cell_volume                     15663.1(10)
_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 0.994
_diffrn_measured_fraction_theta_max 0.996
_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  0.0433
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            70671
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.601
_diffrn_reflns_theta_min         5.144
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.706
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.6613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0674 before and 0.0518 after correction.
The Ratio of minimum to maximum transmission is 0.8782.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.967
_exptl_crystal_description       plate
_exptl_crystal_F_000             4513
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.183
_refine_diff_density_min         -1.042
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5367
_refine_ls_number_restraints     203
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0681
_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^)+(0.1126P)^2^+67.4068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2147
_refine_ls_wR_factor_ref         0.2183
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5054
_reflns_number_total             5367
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b00450_si_005.cif
_cod_data_source_block           Y-pek-MOF-2
_cod_original_cell_volume        15663.1(13)
_cod_original_formula_sum        'C270 H209 F6 N11 O187.50 Y27'
_cod_database_code               4129323
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.606
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Y7, O1}
3. Restrained distances
 C00Z-C00J
 1.5 with sigma of 0.02
 O16-C00J = O15-C00J
 1.26 with sigma of 0.02
 C45-O30B
 1.26 with sigma of 0.02
 C40-C39
 1.5 with sigma of 0.02
 C52-C45
 1.5 with sigma of 0.02
 C43-C43_$1
 2.4 with sigma of 0.02
 C44-C40
 2.78 with sigma of 0.02
 C39-O28
 1.26 with sigma of 0.02
 O28-O28_$1
 2.21 with sigma of 0.02
 C40-O28
 2.37 with sigma of 0.02
 O28-C30 = O29-C30
 1.26 with sigma of 0.02
 C42-C40 = C43-C42 = C44-C43
 1.39 with sigma of 0.02
 C42-C42_$1
 2.4 with sigma of 0.02
 C43-C42_$1
 2.78 with sigma of 0.02
 C42-C39
 2.5 with sigma of 0.02
 F31-C42
 1.34 with sigma of 0.01
 C56-O47
 1.26 with sigma of 0.02
 N1-C56
 1.32 with sigma of 0.02
 N1-O47
 2.26 with sigma of 0.02
 O44-C59
 1.23 with sigma of 0.02
 N39-C59
 1.32 with sigma of 0.02
 N39-O44
 2.26 with sigma of 0.02
 C59-C60
 2.41 with sigma of 0.02
 C61-C59
 2.41 with sigma of 0.02
 C61-C60
 2.47 with sigma of 0.02
 N39-C61
 1.45 with sigma of 0.02
 N1-C57
 1.45 with sigma of 0.02
 N1-C58
 1.45 with sigma of 0.02
 C57-C58
 2.47 with sigma of 0.02
 C58-C56
 2.41 with sigma of 0.02
 C56-C57
 2.41 with sigma of 0.02
 C52-O30B
 2.37 with sigma of 0.02
 C52-C54
 2.78 with sigma of 0.02
 O30A-C55
 1.23 with sigma of 0.02
 C53-C53_$2
 2.4 with sigma of 0.02
 C52-F32
 2.34 with sigma of 0.02
 C53-F32
 2.34 with sigma of 0.02
 C52-C51 = C53-C51 = C54-C53
 1.39 with sigma of 0.02
 C51-C45
 2.5 with sigma of 0.02
 C52-C53 = C51-C54
 2.4 with sigma of 0.02
 C51-F32
 1.34 with sigma of 0.02
 C62-C63
 2.47 with sigma of 0.02
 C63-C55
 2.41 with sigma of 0.02
 C55-C62
 2.41 with sigma of 0.02
 N40-C55
 1.32 with sigma of 0.02
 N40-O30A
 2.26 with sigma of 0.02
 N40-C63 = N40-C62
 1.45 with sigma of 0.02
4. Restrained planarity
 C60, N39, C59, O44, C61
 with sigma of 0.1
 O47, N1, C56, C58, C57
 with sigma of 0.01
 O30B, C45, C51, C53, C54, C52
 with sigma of 0.01
 O30A, C55, N40, C62, C63
 with sigma of 0.01
5. Rigid bond restraints
 C10, C2, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O30B, C45, O30A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O28, O29, C30, C39
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F31, C39, C42, C43, C40, C44
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C45, C51, C53, C54, C52, F32
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Uiso/Uaniso restraints and constraints
C10 \\sim C2 \\sim C15: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
O30B \\sim C45 \\sim O30A: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O28 \\sim O29 \\sim C30 \\sim C39 \\sim O53: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
F31 \\sim C39 \\sim C42 \\sim C43 \\sim C40 \\sim C44: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
O47 \\sim N1 \\sim C56 \\sim C58 \\sim C57: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C60 \\sim N39: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C45 \\sim C51 \\sim C53 \\sim C54 \\sim C52 \\sim F32: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
O30A \\sim C55 \\sim N40: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
O30A \\sim C55 \\sim N40 \\sim C62 \\sim C63: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
Uanis(O51) \\sim Ueq, Uanis(O52) \\sim Ueq: with sigma of 0.0025 and sigma for
terminal atoms of 0.005
Uanis(Y7) = Uanis(O1)
7. Others
 Fixed Sof: Y7(0.25) Y8(0.125) O49B(0.25) C00J(0.5) O15(0.5) O16(0.5)
 O13(0.125) C10(0.5) C2(0.5) H2(0.5) C15(0.5) H15(0.5) C00Z(0.5) C26(0.5)
 H26(0.5) C29(0.5) H29(0.5) C19(0.5) H19A(0.5) H19B(0.5) O30B(0.25) O28(0.375)
 O29(0.125) C30(0.125) F31(0.125) C39(0.125) O36(0.25) O37(0.25) O0AA(0.25)
 O7(0.125) C42(0.25) H31(0.125) C43(0.25) H43(0.25) C40(0.125) C44(0.125)
 H44(0.125) C45(0.125) O30A(0.25) C51(0.25) H51(0.125) C53(0.25) H53(0.25)
 C54(0.125) H54(0.125) C52(0.125) F32(0.125) C60(0.25) H60A(0.25) H60B(0.25)
 H60C(0.25) N39(0.25) C59(0.25) H59(0.25) O42(0.0625) O44(0.25) O45(0.02083)
 O46(0.0625) O47(0.08333) O1(0.25) O53(0.125) O54(0.125) C55(0.125) H29A(0.125)
 N1(0.08333) C56(0.08333) H56(0.08333) C58(0.08333) H58A(0.08333) H58B(0.08333)
 H58C(0.08333) C57(0.08333) H57A(0.08333) H57B(0.08333) H57C(0.08333) C61(0.25)
 H61A(0.25) H61B(0.25) H61C(0.25) N40(0.125) C62(0.125) H62A(0.125) H62B(0.125)
 H62C(0.125) C63(0.125) H63A(0.125) H63B(0.125) H32(0.125)
8.a Riding coordinates:
 C42(H31), C43(H43), C44(H44), C51(H51), C53(H53), C60(H60A,H60B,H60C),
 C58(H58A,H58B,H58C), C57(H57A,H57B,H57C), C61(H61A,H61B,H61C)
8.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B)
8.c Me refined with riding coordinates:
 C62(H62A,H62B,H62C), C63(H63A,H63B,H32)
8.d Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C18(H18), C2(H2), C15(H15), C26(H26), C29(H29), C54(H54),
 C59(H59), C55(H29A), C56(H56)
8.e Fitted hexagon refined as free rotating group:
 C10(C2,C15,C00Z,C26,C29)
;
_olex2_submission_special_instructions 'No special instructions were received'