Rare Earth pcu MOF Platform Based on RE4(μ3-OH)4(COO)62+ Clusters: Rational Design, Directed Synthesis, and Deliberate Tuning of Excitation Wavelengths.
Luo, Tian-Yi; Liu, Chong; Eliseeva, Svetlana V.; Muldoon, Patrick Flynn; Petoud, Stephane; Rosi, Nathaniel L.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b04532

data_4126253
_publ_section_title
;
 Rare Earth pcu MOF Platform Based on RE4(\m3-OH)4(COO)62+ Clusters:
 Rational Design, Directed Synthesis, and Deliberate Tuning of Excitation
 Wavelengths.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b04532
_journal_year                    2017
_chemical_formula_moiety         'C60.73 H47.04 Dy4 N9.58 O24'
_chemical_formula_sum            'C60.73 H47.05 Dy4 N9.58 O24'
_chemical_formula_weight         1945.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.864(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0453(8)
_cell_length_b                   18.1800(8)
_cell_length_c                   32.5984(14)
_cell_measurement_reflns_used    9802
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      51.45
_cell_measurement_theta_min      3.460
_cell_volume                     10638.4(8)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      240.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8
_diffrn_detector_type            'APEX II CCD'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker X8 Prospector Ultra'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1098
_diffrn_reflns_av_unetI/netI     0.0990
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            46081
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        51.444
_diffrn_reflns_theta_max         51.444
_diffrn_reflns_theta_min         2.725
_diffrn_source                   'IMuS micro-focus source'
_diffrn_source_target            Cu
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.237
_exptl_absorpt_correction_T_max  0.7501
_exptl_absorpt_correction_T_min  0.3206
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1501 before and 0.0792 after correction.
The Ratio of minimum to maximum transmission is 0.4274.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_description       rectanglar
_exptl_crystal_F_000             3738
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.307
_refine_diff_density_min         -2.252
_refine_diff_density_rms         0.274
_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     860
_refine_ls_number_reflns         11485
_refine_ls_number_restraints     1074
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.1303
_refine_ls_R_factor_gt           0.1099
_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^)+(0.0973P)^2^+504.2673P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2814
_refine_ls_wR_factor_ref         0.2939
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8979
_reflns_number_total             11485
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b04532_si_004.cif
_cod_data_source_block           lty2771_0m_a
_cod_database_code               4126253
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.462
_shelx_estimated_absorpt_t_min   0.262
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C35-N6B
 1.38 with sigma of 0.02
 C49-N2B
 1.38 with sigma of 0.02
 C54-N1A
 1.38 with sigma of 0.02
 C17-N7A
 1.38 with sigma of 0.02
 C10-N3
 1.38 with sigma of 0.02
 C34-N6B
 2.36 with sigma of 0.04
 C48-N2B
 2.36 with sigma of 0.04
 C55-N1A
 2.36 with sigma of 0.04
 C18-N7A
 2.36 with sigma of 0.04
 C45-N2A \\sim C49-N2B
 with sigma of 0.02
 C46-N2A \\sim C48-N2B
 with sigma of 0.02
 C31-N6A \\sim C35-N6B
 with sigma of 0.02
 C32-N6A \\sim C34-N6B
 with sigma of 0.02
 C17-N7A \\sim C21-N7B
 with sigma of 0.02
 C18-N7A \\sim C20-N7B
 with sigma of 0.02
 N61S-C63S \\sim N61S-C62S
 with sigma of 0.02
 C61S-C63S \\sim C61S-C62S
 with sigma of 0.02
3. Restrained planarity
 C52, C53, C54, N1A, N1B
 with sigma of 0.1
 C44, C45, C49, N2A, N2B
 with sigma of 0.1
 C30, C31, C35, N6A, N6B
 with sigma of 0.1
 C16, C17, C21, N7A, N7B
 with sigma of 0.1
 N91S, C91S, C92S, C93S
 with sigma of 0.1
 N81S, C81S, C82S, C83S
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O15 \\sim O16 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim
C56 \\sim N1A \\sim N1B: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim N2A \\sim N2B:
within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim N6A \\sim N6B:
within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim N7A \\sim N7B:
within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
O61S \\sim N61S \\sim C61S \\sim C62S \\sim C63S: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
O91S \\sim N91S \\sim C91S \\sim C92S \\sim C93S: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
O81S \\sim N81S \\sim C81S \\sim C82S \\sim C83S: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
N8 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
N5 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
N4 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
N3 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
O19 \\sim O20 \\sim C28: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
O11 \\sim O12 \\sim C42: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
O13 \\sim O14 \\sim C43: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
O17 \\sim O18 \\sim C15: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
O5 \\sim O6 \\sim C1: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(O2) = Uanis(O4) = Uanis(O1)
Uanis(C49) = Uanis(C45) = Uanis(C46)
5. Rigid body (RIGU) restrains
 O15, O16, C50, C51, C52, C53, C54, C55, C56, N1A, N1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C44, C45, C46, C47, C48, C49, N2A, N2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C30, C31, C32, C33, C34, C35, N6A, N6B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C16, C17, C18, C19, C20, C21, N7A, N7B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O61S, N61S, C61S, C62S, C63S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O91S, N91S, C91S, C92S, C93S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O81S, N81S, C81S, C82S, C83S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N8, C22, C23, C24, C25, C26, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N5, C36, C37, C38, C39, C40, C41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4, C2, C3, C4, C5, C6, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N3, C8, C9, C10, C11, C12, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O19, O20, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O11, O12, C42
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O13, O14, C43
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O17, O18, C15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, O6, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(N1B)=Sof(H1BA)=Sof(H1BB)=1-FVAR(1)
 Sof(N1A)=Sof(H1AA)=Sof(H1AB)=FVAR(1)
 Sof(N2B)=Sof(H2BA)=Sof(H2BB)=1-FVAR(2)
 Sof(N2A)=Sof(H2AA)=Sof(H2AB)=FVAR(2)
 Sof(N6B)=Sof(H6BA)=Sof(H6BB)=1-FVAR(3)
 Sof(N6A)=Sof(H6AA)=Sof(H6AB)=FVAR(3)
 Sof(N7B)=Sof(H7BA)=Sof(H7BB)=1-FVAR(4)
 Sof(N7A)=Sof(H7AA)=Sof(H7AB)=FVAR(4)
 Sof(N61S)=Sof(C61S)=Sof(H61S)=Sof(C62S)=Sof(H62A)=Sof(H62B)=Sof(H62C)=
 Sof(C63S)=Sof(H63A)=Sof(H63B)=Sof(H63C)=FVAR(5)
 Sof(N81S)=Sof(C81S)=Sof(H81S)=Sof(C82S)=Sof(H82A)=Sof(H82B)=Sof(H82C)=
 Sof(C83S)=Sof(H83A)=Sof(H83B)=Sof(H83C)=FVAR(6)
 Sof(N91S)=Sof(C91S)=Sof(H91S)=Sof(C92S)=Sof(H92A)=Sof(H92B)=Sof(H92C)=
 Sof(C93S)=Sof(H93A)=Sof(H93B)=Sof(H93C)=FVAR(7)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C9(H9), C12(H12), C13(H13), C18(H18), C20(H20),
 C23(H23), C24(H24), C27(H27), C32(H32), C34(H34), C37(H37), C38(H38), C41(H41),
  C46(H46), C48(H48), C51(H51), C55(H55), C81S(H81S), C91S(H91S), C61S(H61S)
7.b Fitted hexagon refined as free rotating group:
 C2(C3,C4,C5,C6,C7), C8(C9,C10,C11,C12,C13), C16(C17,C18,C19,C20,C21), C22(C23,
 C24,C25,C26,C27), C30(C31,C32,C33,C34,C35), C36(C37,C38,C39,C40,C41), C44(C45,
 C46,C47,C48,C49), C50(C51,C52,C53,C54,C55)
7.c X=CH2 refined with riding coordinates:
 N3(H3A,H3B), N4(H4A,H4B), N5(H5A,H5B), N8(H8A,H8B), N1A(H1AA,H1AB), N2A(H2AA,
 H2AB), N6A(H6AA,H6AB), N7A(H7AA,H7AB), N1B(H1BA,H1BB), N2B(H2BA,H2BB),
 N6B(H6BA,H6BB), N7B(H7BA,H7BB)
7.d Idealised Me refined with everything fixed:
 C82S(H82A,H82B,H82C), C83S(H83A,H83B,H83C), C92S(H92A,H92B,H92C), C93S(H93A,
 H93B,H93C), C62S(H62A,H62B,H62C), C63S(H63A,H63B,H63C)
;
_shelx_res_checksum              51288
_shelx_hkl_checksum              38921
_olex2_submission_special_instructions 'No special instructions were received'