Enhancing magnetic relaxation through subcomponent self-assembly from a Dy2 to Dy4 grid
Li, Xiao-Lei; Ma, Zhifang; Wu, Jinjiang; Zhou, Quan; Tang, Jinkui; Dalton Transactions  (2022) –; doi:10.1039/D2DT02996K

data_7711700
_publ_section_title
;
 Enhancing magnetic relaxation through subcomponent self-assembly from a
 Dy2 to Dy4 grid
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02996K
_journal_year                    2022
_chemical_formula_moiety
'C97 H83 Dy4 N12 Na2 O28, 2(C2 H3 N), C H4 O, 7(H2 O), 1[CH4O], 1[H2O], 1[CH4O], 2[H2O]'
_chemical_formula_sum            'C104 H121 Dy4 N14 Na2 O41'
_chemical_formula_weight         2919.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-19
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2022-10-20 deposited with the CCDC.	2022-10-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.5540(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.3852(6)
_cell_length_b                   32.5128(16)
_cell_length_c                   15.4534(7)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.04
_cell_measurement_theta_min      2.25
_cell_volume                     5964.8(5)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_collection       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.1045
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37654
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.075
_diffrn_reflns_theta_min         1.511
_exptl_absorpt_coefficient_mu    2.572
_exptl_absorpt_correction_T_max  0.599
_exptl_absorpt_correction_T_min  0.468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0635 before and 0.0485 after correction.
The Ratio of minimum to maximum transmission is 0.8363.
The \l/2 correction factor is 0.0013.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_description       block
_exptl_crystal_F_000             2914
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.634
_refine_diff_density_min         -1.217
_refine_diff_density_rms         0.159
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.379(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1418
_refine_ls_number_reflns         23472
_refine_ls_number_restraints     1846
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0514P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1302
_reflns_Friedel_coverage         0.958
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                17944
_reflns_number_total             23472
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02996k2.cif
_cod_data_source_block           Dy4Na2
_cod_database_code               7711700
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.627
_shelx_estimated_absorpt_t_min   0.512
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.62119
 0.37881
2. Restrained distances
 H18A-O18
 0.8 with sigma of 0.02
 C100-O26
 1.6 with sigma of 0.02
 H13-O13
 0.8 with sigma of 0.02
 C1A-N14
 1.137 with sigma of 0.01
 C1B-N14
 2.593 with sigma of 0.02
 C1A-C1B
 1.456 with sigma of 0.01
 N14-C1A
 1.14 with sigma of 0.02
 H33B-H67
 2.1 with sigma of 0.02
 N14-C1B
 2.59 with sigma of 0.04
 C32-C91 \\sim C32-C114
 with sigma of 0.02
 C90-C91 \\sim C113-C114
 with sigma of 0.02
 C90-C95 \\sim C113-C112
 with sigma of 0.02
 C91-C92 \\sim C114-C109
 with sigma of 0.02
 C92-C93 \\sim C109-C110
 with sigma of 0.02
 C93-C94 \\sim C110-C111
 with sigma of 0.02
 C94-C95 \\sim C111-C112
 with sigma of 0.02
 C32-C90 \\sim C32-C113
 with sigma of 0.04
 C32-C92 \\sim C32-C109
 with sigma of 0.04
 C90-C92 \\sim C113-C109
 with sigma of 0.04
 C90-C94 \\sim C113-C111
 with sigma of 0.04
 C91-C93 \\sim C114-C110
 with sigma of 0.04
 C91-C95 \\sim C114-C112
 with sigma of 0.04
 C92-C94 \\sim C109-C111
 with sigma of 0.04
 C93-C95 \\sim C110-C112
 with sigma of 0.04
 C43-C87 \\sim C43-C103
 with sigma of 0.02
 C84-C85 \\sim C106-C107
 with sigma of 0.02
 C84-C89 \\sim C106-C105
 with sigma of 0.02
 C85-C86 \\sim C107-C108
 with sigma of 0.02
 C86-C87 \\sim C108-C103
 with sigma of 0.02
 C87-C88 \\sim C103-C104
 with sigma of 0.02
 C88-C89 \\sim C104-C105
 with sigma of 0.02
 C43-C86 \\sim C43-C108
 with sigma of 0.04
 C43-C88 \\sim C43-C104
 with sigma of 0.04
 C84-C86 \\sim C106-C108
 with sigma of 0.04
 C84-C88 \\sim C106-C104
 with sigma of 0.04
 C85-C87 \\sim C107-C103
 with sigma of 0.04
 C85-C89 \\sim C107-C105
 with sigma of 0.04
 C86-C88 \\sim C108-C104
 with sigma of 0.04
 C87-C89 \\sim C103-C105
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C51: within 3.8A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
C46 \\sim C38 \\sim C73 \\sim C70 \\sim C76 \\sim C58: within 3.8A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
N14 \\sim C1A \\sim C1B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C114 \\sim C109 \\sim C110 \\sim C111 \\sim C112 \\sim C113: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
O19 \\sim C97: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3.8A
C79 \\sim C80 \\sim C81 \\sim C82 \\sim C83 \\sim C78: within 3.8A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
C3 \\sim C25 \\sim C12 \\sim C31 \\sim C40 \\sim C2 \\sim O19 \\sim C97: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
Uanis(C36) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C109) \\sim Ueq, Uanis(C86) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O38) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C96, O3, O13, O8, O2, O11, N1, O7, N4, O4, C29, C13, Na1, C3, H13, C26, C10,
 C11, N3, C9, C46, C22, O9, O19, O26, O27, C2, C25, O1, O10, O17, N5, N6, C4,
 C33, H10A, N2, C44, H3, H9, C38, C58, C37, C39, C14, C97, C100, C15, C77, C40,
 C12, C6, C24, N10, C23, C21, C62, C20, C5, H44, H38, C73, H58, C76, H37, C66,
 H39, C69, C19, H97A, H97B, H97C, C16, H77A, H77B, H77C, C31, H40, H12, H6, N12,
  C1, H10, H23, C42, C67, C61, H62, H20, C59, O20, O18, O22, O25, O24, O16, N11,
  C32, O12, C43, Na2, N8, C70, H73, H76, H66, C75, H69, C18, H16, C17, H31, C7,
 H1, H42, C64, H67, C48, H61, C65, H59, C72, H18A, C36, C68, C91, C114, C87,
 C103, O15, O21, O23, O28, H8, H70, H75, H18, H17, O6, O14, O5, N9, C8, N7, C49,
  H64, H48, H65, C28, C63, C30, H68, C90, C92, C109, C113, C86, C88, C104, C108,
  C74, C79, C78, H28A, H28B, C41, C52, H7, H49, C71, C47, C27, C101, H90, C95,
 H92, C93, H109, C110, C112, H113, C85, H86, H88, C89, H104, C105, C107, H108,
 H74A, H74B, H74C, C80, C83, H96A, H96B, H96C, H41, C51, C53, H71, C60, H47,
 H27, C45, H101, C50, C94, H95, H93, H110, C111, H112, C84, H85, H89, H105,
 C106, H107, C81, C82, H83, H51, C56, H53, C54, H60, H45, C57, H50, H94, H111,
 H84, H106, H81, H82, C55, H56, H54, H57, H55
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N14, C1A, C1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C99, C98, N13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C103)=Sof(C104)=Sof(H104)=Sof(C105)=Sof(H105)=Sof(C106)=Sof(H106)=
 Sof(C107)=Sof(H107)=Sof(C108)=Sof(H108)=1-FVAR(1)
 Sof(C84)=Sof(H84)=Sof(C85)=Sof(H85)=Sof(C86)=Sof(H86)=Sof(C87)=Sof(C88)=
 Sof(H88)=Sof(C89)=Sof(H89)=FVAR(1)
 Sof(C109)=Sof(H109)=Sof(C110)=Sof(H110)=Sof(C111)=Sof(H111)=Sof(C112)=
 Sof(H112)=Sof(C113)=Sof(H113)=Sof(C114)=1-FVAR(2)
 Sof(C90)=Sof(H90)=Sof(C91)=Sof(C92)=Sof(H92)=Sof(C93)=Sof(H93)=Sof(C94)=
 Sof(H94)=Sof(C95)=Sof(H95)=FVAR(2)
6.a Everything fixed:
 O13, H13, O18, H18A, O28, H28A, H28B, O29, H29, O31, H31A, H31B, O32, H32A,
 H32B, O30, H30A, H30B, O33, H33A, H33B, O38, H38A, H38B
6.b Riding coordinates:
 C99(H99A,H99B,H99C)
6.c Free rotating group:
 O36(H36A,H36B), O37(H37A,H37B)
6.d Aromatic/amide H refined with riding coordinates:
 C1(H1), N3(H3), C6(H6), N7(H7), N8(H8), C9(H9), N10(H10), C10(H10A), C12(H12),
  C16(H16), C17(H17), C18(H18), C20(H20), C23(H23), C31(H31), C27(H27),
 C101(H101), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
 C44(H44), C45(H45), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C53(H53),
  C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60),
 C61(H61), C62(H62), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68), C69(H69),
  C70(H70), C71(H71), C73(H73), C75(H75), C76(H76), C81(H81), C82(H82),
 C83(H83), C84(H84), C85(H85), C86(H86), C88(H88), C89(H89), C90(H90), C92(H92),
  C93(H93), C94(H94), C95(H95), C104(H104), C105(H105), C106(H106), C107(H107),
 C108(H108), C109(H109), C110(H110), C111(H111), C112(H112), C113(H113)
6.e Fitted hexagon refined as free rotating group:
 C84(C85,C86,C87,C88,C89), C90(C91,C92,C93,C94,C95), C103(C104,C105,C106,C107,
 C108), C109(C110,C111,C112,C113,C114)
6.f Idealised Me refined as rotating group:
 C74(H74A,H74B,H74C), C77(H77A,H77B,H77C), C96(H96A,H96B,H96C), C97(H97A,H97B,
 H97C), C100(H10B,H10C,H10D), C102(H10E,H10F,H10G), C1B(H1BA,H1BB,H1BC)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 132 electrons were 
found in a volume of 648\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 2[CH4O] and 3[H2O]
per Formula Unit which account for 132 electrons per unit cell.
;
_shelx_res_checksum              72068
_shelx_hkl_checksum              95916
_shelx_fab_checksum              97913
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'