Facile and environmentally friendly synthesis of six heterometallic dumbbell-shaped MLn (M = Co, Ni; Ln = Eu, Gd, Dy) clusters as cryogenic magnetic coolants and molecular magnets.
Shao, Feng; Zhuang, Jia-Jia; Chen, Ming-Guang; Wang, Ning; Shi, Hai-Yan; Tong, Jia-Ping; Luo, Gang; Tao, Jun; Zheng, Lan-Sun; Dalton transactions (Cambridge, England : 2003) 47 (2018) 16850–16854; doi:10.1039/c8dt04153a

data_7048157
_publ_section_title
;
 Facile and environmentally friendly synthesis of six heterometallic
 dumbbell-shaped MLn (M = Co, Ni; Ln = Eu, Gd, Dy) clusters as cryogenic
 magnetic coolants and molecular magnets.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16850
_journal_page_last               16854
_journal_paper_doi               10.1039/c8dt04153a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'C36 H74 Dy4 N3 Ni5 O45, 2(C H4 O), C H3 O, 0.67(C O)'
_chemical_formula_sum            'C39.67 H96.17 Dy4 N3 Ni5 O48.67'
_chemical_formula_weight         2337.60
_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   mixed
_audit_creation_date             2018-11-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-03 deposited with the CCDC.
2018-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.082(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2406(2)
_cell_length_b                   28.2759(4)
_cell_length_c                   21.0581(5)
_cell_measurement_reflns_used    7598
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      60.7520
_cell_measurement_theta_min      3.7870
_cell_volume                     7736.9(2)
_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-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_av_unetI/netI     0.0876
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22582
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        60.168
_diffrn_reflns_theta_max         60.168
_diffrn_reflns_theta_min         3.126
_exptl_absorpt_coefficient_mu    22.414
_exptl_absorpt_correction_T_max  0.4009
_exptl_absorpt_correction_T_min  0.0943
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.007
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4594
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.324
_refine_diff_density_min         -1.418
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         11400
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0799
_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^)+(0.0832P)^2^+138.9966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1919
_refine_ls_wR_factor_ref         0.2114
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8723
_reflns_number_total             11400
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04153a2.cif
_cod_data_source_block           6_Ni5Dy4
_cod_depositor_comments
'Adding full bibliography for 7048154--7048159.cif.'
_cod_database_code               7048157
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.400
_shelx_estimated_absorpt_t_min   0.094
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, H46 of O46, H35 of O35, H33 of O33
 At 1.2 times of:
  H47 of O47
2. Restrained distances
 C7-O7
 1.44 with sigma of 0.01
 O1AA-O36
 3 with sigma of 0.02
 O33-H33
 0.85 with sigma of 0.01
 O35-H35
 0.85 with sigma of 0.01
 C33-H33
 1.881442 with sigma of 0.02
 Dy2-H33
 2.876551 with sigma of 0.02
 C35-H35
 1.908256 with sigma of 0.02
 Dy3-H35
 2.836553 with sigma of 0.02
3. Rigid bond restraints
 C34, O34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, O2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C7, O7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C34) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C1AA) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Fixed Sof: C0AA(0.66667) C1AA(0.33333) O1AA(0.66667) C2AA(0.66667)
6.a Riding coordinates:
 O47(H47)
6.b Me refined with riding coordinates:
 C4(H4A,H4B,H4C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C1(H1A,H1B,H1C), C6(H6A,
 H6B,H6C), C22(H22A,H22B,H22C), C33(H33A,H33B,H33C), C8(H8A,H8B,H8C), C16(H16A,
 H16B,H16C), C20(H20A,H20B,H20C), C32(H32A,H32B,H32C), C10(H10A,H10B,H10C),
 C12(H12A,H12B,H12C), C24(H24A,H24B,H24C), C28(H28A,H28B,H28C), C14(H14A,H14B,
 H14C), C29(H29A,H29B,H29C), C2(H2A,H2B,H2C), C31(H31A,H31B,H31C), C26(H26A,
 H26B,H26C), C18(H18A,H18B,H18C), C35(H35A,H35B,H35C), C34(H34A,H34B,H34C),
 C7(H7A,H7B,H7C)
6.c Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C)
6.d Idealised tetrahedral OH refined as rotating group:
 O46(H46)
;
_shelx_res_checksum              60169
_olex2_submission_special_instructions 'No special instructions were received'