A Dy4 single-molecule magnet and its Gd(iii), Tb(iii), Ho(iii), and Er(iii) analogues encapsulated by an 8-hydroxyquinoline Schiff base derivative and β-diketonate coligand.
Gao, Hong-Ling; Zhou, Xiao-Pu; Bi, Yan-Xia; Shen, Hai-Yun; Wang, Wen-Min; Wang, Ni-Ni; Chang, Yi-Xin; Zhang, Ru-Xia; Cui, Jian-Zhong; Dalton transactions (Cambridge, England : 2003) 46 (2017) 4669–4677; doi:10.1039/c7dt00118e

data_7042427
_publ_section_title
;
 A Dy4 single-molecule magnet and its Gd(iii), Tb(iii), Ho(iii), and
 Er(iii) analogues encapsulated by an 8-hydroxyquinoline Schiff base
 derivative and \b-diketonate coligand.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4669
_journal_page_last               4677
_journal_paper_doi               10.1039/c7dt00118e
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C116 H96 Er4 N12 O16, C2 H3 N, 0.25(C2 Cl4)'
_chemical_formula_sum            'C118.5 H99 Cl Er4 N13 O16'
_chemical_formula_weight         2665.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-02-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-02-10 deposited with the CCDC.
2017-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.165(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.4688(19)
_cell_length_b                   14.5825(6)
_cell_length_c                   28.1141(17)
_cell_measurement_reflns_used    12535
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     11012.3(15)
_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      113.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            58628
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.019
_diffrn_reflns_theta_max         25.019
_diffrn_reflns_theta_min         3.033
_exptl_absorpt_coefficient_mu    3.112
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             5272
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.173
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     726
_refine_ls_number_reflns         9695
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+71.6117P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0849
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8311
_reflns_number_total             9695
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00118e2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7042423--7042427.cif.'
_cod_original_formula_sum        'C118.50 H99 Cl Er4 N13 O16'
_cod_database_code               7042427
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.789
_shelx_estimated_absorpt_t_min   0.746
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C61-N7
 2.66 with sigma of 0.01
 C60-C61
 1.54 with sigma of 0.01
 C60-N7
 1.12 with sigma of 0.01
 Cl1-Cl2
 2.8 with sigma of 0.01
 C59-Cl1 = C59-Cl2
 1.78 with sigma of 0.01
 H22-H61A
 2.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim C59: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C61) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C59)
\\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(Cl2) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: N7(0.5) C60(0.5) C61(0.5) H61A(0.5) H61B(0.5) H61C(0.5) Cl1(0.25)
 Cl2(0.25) C59(0.25)
5.a Ternary CH refined with riding coordinates:
 O8(H8)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23),
  C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
 C34(H34), C35(H35), C38(H38), C39(H39), C42(H42), C44(H44), C45(H45), C46(H46),
  C47(H47), C48(H48), C51(H51), C56(H56)
5.c Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C58(H58A,H58B,
 H58C), C61(H61A,H61B,H61C)
;
_shelx_res_checksum              41838
_olex2_submission_special_instructions 'No special instructions were received'