A new air- and moisture-stable pentagonal-bipyramidal Dy<sup>III</sup> single-ion magnet based on the HMPA ligand.
Li, Lei-Lei; Su, Hong-Dan; Liu, Shuang; Xu, Ya-Chao; Wang, Wen-Zhen; Dalton transactions (Cambridge, England : 2003) 48 (2019) 2213–2219; doi:10.1039/c8dt03565b

data_7048451
_publ_section_title
;
 A new air- and moisture-stable pentagonal-bipyramidal Dy<sup>III</sup>
 single-ion magnet based on the HMPA ligand.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2213
_journal_page_last               2219
_journal_paper_doi               10.1039/c8dt03565b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'C12 H46 Dy N6 O7 P2, 3(Br), C6 H18 N3 O P, H2 O'
_chemical_formula_sum            'C18 H66 Br3 Dy N9 O9 P3'
_chemical_formula_weight         1047.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc201mc2
_audit_creation_date             2018-06-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-11 deposited with the CCDC.
2019-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.509(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.6240(17)
_cell_length_b                   39.353(6)
_cell_length_c                   19.919(3)
_cell_measurement_reflns_used    1282
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      18.18
_cell_measurement_theta_min      2.15
_cell_volume                     8929(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1608
_diffrn_reflns_av_unetI/netI     0.2131
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44601
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         1.165
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.511
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0910 before and 0.0652 after correction.
The Ratio of minimum to maximum transmission is 0.7789.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_description       prism
_exptl_crystal_F_000             4200
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.420
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     952
_refine_ls_number_reflns         15731
_refine_ls_number_restraints     486
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.2067
_refine_ls_R_factor_gt           0.0707
_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^)+(0.0494P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1774
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6133
_reflns_number_total             15731
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03565b2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7048451.cif.'
_cod_database_code               7048451
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.466
_shelx_estimated_absorpt_t_min   0.173
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All N(H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 N15-C1P = N15-C1O
 1.49 with sigma of 0.02
 C1P-C1O
 2.5 with sigma of 0.02
 C1O-C1P = C1Q-C0AA = C1AA-C4A = C4-C1M = C12-C1N
 2.5 with sigma of 0.02
 P1-N12A = P1-N12 = P1-N15A = P1-N15 = P1-N13A = P1-N13
 1.62 with sigma of 0.02
 N15-C1O = N15A-C0AA = N15A-C1Q = N15-C1P = N13A-C12A = N13-C12 = N13-C1N =
 N12A-C4A = N12A-C1AA = N12-C1M = N12-C4
 1.5 with sigma of 0.02
 N13A-C2AA
 1.4 with sigma of 0.02
 C2AA-C12A
 2.5 with sigma of 0.02
 C2AA-C1Q
 2.6 with sigma of 0.01
 N20A-C4AA = N20A-C3AA = N20-C1F = N20-C1D
 1.5 with sigma of 0.02
 P2-N20 = P2-N20A
 1.6 with sigma of 0.02
 H12A-Br1
 2.6 with sigma of 0.02
 H14A-Br4
 2.6 with sigma of 0.02
 O14-H14B
 0.9 with sigma of 0.02
 O19-H19B
 0.9 with sigma of 0.02
 H13A-Br3
 2.5 with sigma of 0.02
 H11A-Br2_$1
 2.5 with sigma of 0.02
 O11-H11B
 0.9 with sigma of 0.02
 H11B-H1E
 1.96 with sigma of 0.02
 H15B-Br4
 2.5 with sigma of 0.02
 H8D-H12E
 2.77 with sigma of 0.02
 H8E-Br3
 2.6 with sigma of 0.02
 H15A-H8E
 2.2 with sigma of 0.02
 P2-N20A \\sim P2-N20
 with sigma of 0.02
 N20A-C4AA \\sim N20A-C3AA \\sim N20-C1F \\sim N20-C1D
 with sigma of 0.02
 C4AA-C3AA \\sim C1F-C1D
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C6 \\sim N16 \\sim C1G \\sim N10 \\sim C15 \\sim C1B \\sim C1A \\sim N8 \\sim
C18 \\sim P4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C1O \\sim C0AA: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
N15 \\sim N15A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C1P \\sim C1Q: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C1M \\sim C1AA: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
N12 \\sim N12A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C4 \\sim C4A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C1N: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
N13 \\sim N13A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C12 \\sim C12A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
P1 \\sim N12 \\sim N15 \\sim N13 \\sim C4 \\sim C12 \\sim C1M \\sim C1N \\sim
C1O \\sim C1P \\sim C0AA \\sim N15A \\sim C1Q \\sim C1AA \\sim N12A \\sim C4A
\\sim N13A \\sim C12A \\sim C2AA: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C11 \\sim C1E \\sim N18: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Br2 \\sim P3 \\sim N5 \\sim N9 \\sim N11 \\sim C20 \\sim C2 \\sim C1 \\sim C1C
\\sim C1H \\sim C19: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08
C1J \\sim N2: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
C4AA \\sim C1F \\sim C1D \\sim C3AA \\sim N20 \\sim N20A \\sim P2: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=Sof(N15A)=Sof(C1Q)=Sof(H1QA)=
 Sof(H1QB)=Sof(H1QC)=Sof(C1AA)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(N12A)=Sof(C4A)=
 Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=Sof(N13A)=Sof(C12A)=Sof(H12F)=Sof(H12G)=
 Sof(H12H)=Sof(C2AA)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=1-FVAR(1)
 Sof(N12)=Sof(N15)=Sof(N13)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C12)=
 Sof(H12C)=Sof(H12D)=Sof(H12E)=Sof(C1M)=Sof(H1MA)=Sof(H1MB)=Sof(H1MC)=Sof(C1N)=
 Sof(H1NA)=Sof(H1NB)=Sof(H1NC)=Sof(C1O)=Sof(H1OA)=Sof(H1OB)=Sof(H1OC)=Sof(C1P)=
 Sof(H1PA)=Sof(H1PB)=Sof(H1PC)=FVAR(1)
 Sof(C3AA)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C4AA)=Sof(H4AD)=Sof(H4AE)=
 Sof(H4AF)=Sof(N20A)=1-FVAR(2)
 Sof(N20)=Sof(C1D)=Sof(H1DA)=Sof(H1DB)=Sof(H1DC)=Sof(C1F)=Sof(H1FA)=Sof(H1FB)=
 Sof(H1FC)=FVAR(2)
5.a Free rotating group:
 O4(H4D,H4E), O8(H8D,H8E)
5.b Rotating group:
 O11(H11A,H11B), O12(H12A,H12B), O13(H13A,H13B), O14(H14A), O15(H15A,H15B),
 O16(H16A,H16B), O17(H17A,H17B), O19(H19A), O20(H20A,H20B), O1(H1D,H1E)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C14(H14C,H14D,H14E), C17(H17C,H17D,H17E),
 C18(H18A,H18B,H18C), C20(H20C,H20D,H20E), C9(H9A,H9B,H9C), C13(H13C,H13D,H13E),
  C2(H2A,H2B,H2C), C16(H16C,H16D,H16E), C3(H3A,H3B,H3C), C19(H19C,H19D,H19E),
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C10(H10A,H10B,H10C),
 C11(H11C,H11D,H11E), C12(H12C,H12D,H12E), C1A(H1AD,H1AE,H1AF), C1B(H1BA,H1BB,
 H1BC), C1(H1A,H1B,H1C), C15(H15C,H15D,H15E), C1C(H1CA,H1CB,H1CC), C1D(H1DA,
 H1DB,H1DC), C1E(H1EA,H1EB,H1EC), C1F(H1FA,H1FB,H1FC), C1G(H1GA,H1GB,H1GC),
 C1H(H1HA,H1HB,H1HC), C1I(H1IA,H1IB,H1IC), C1J(H1JA,H1JB,H1JC), C1K(H1KA,H1KB,
 H1KC), C1L(H1LA,H1LB,H1LC), C1M(H1MA,H1MB,H1MC), C1N(H1NA,H1NB,H1NC), C1O(H1OA,
 H1OB,H1OC), C1P(H1PA,H1PB,H1PC), C0AA(H0AA,H0AB,H0AC), C1Q(H1QA,H1QB,H1QC),
 C1AA(H1AA,H1AB,H1AC), C4A(H4AA,H4AB,H4AC), C12A(H12F,H12G,H12H), C2AA(H2AA,
 H2AB,H2AC), C3AA(H3AA,H3AB,H3AC), C4AA(H4AD,H4AE,H4AF)
;
_olex2_submission_special_instructions 'No special instructions were received'