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_7048154
_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
'C32 H73 Co5 Dy4 N4 O46, C H O, 2(C H4 O), C H3 O'
_chemical_formula_sum            'C36 H87 Co5 Dy4 N4 O50'
_chemical_formula_weight         2320.74
_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                 92.74(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.500(3)
_cell_length_b                   17.702(4)
_cell_length_c                   29.025(6)
_cell_measurement_reflns_used    17518
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      54.99
_cell_measurement_theta_min      6.02
_cell_volume                     7442(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0910
_diffrn_reflns_av_unetI/netI     0.0844
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            51959
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         3.010
_exptl_absorpt_coefficient_mu    5.151
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.071
_exptl_crystal_description       block
_exptl_crystal_F_000             4520
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.773
_exptl_transmission_factor_min   0.302
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.860
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     913
_refine_ls_number_reflns         14510
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0601P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1422
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10188
_reflns_number_total             14510
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04153a2.cif
_cod_data_source_block           3_Co5Dy4
_cod_depositor_comments
'Adding full bibliography for 7048154--7048159.cif.'
_cod_database_code               7048154
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.783
_shelx_estimated_absorpt_t_min   0.232
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, H49 of O49, H48 of O48, H50 of O50, H33 of O33, H32 of
  O32, H31 of O31, H30 of O30
 At 1.2 times of:
  H3 of O3, H7 of O7, H34 of O34
2. Restrained distances
 O34-H34
 0.87 with sigma of 0.01
 O33-H33
 0.87 with sigma of 0.01
 O31-H31
 0.87 with sigma of 0.01
 O32-H32
 0.87 with sigma of 0.01
 O30-H30
 0.87 with sigma of 0.01
 C34-H34
 1.891257 with sigma of 0.02
 Dy4-H34
 2.942676 with sigma of 0.02
 C33-H33
 1.897689 with sigma of 0.02
 Dy3-H33
 2.961787 with sigma of 0.02
 C31-H31
 1.8993 with sigma of 0.02
 Dy2-H31
 2.976323 with sigma of 0.02
 C32-H32
 1.922725 with sigma of 0.02
 Co5-H32
 2.772411 with sigma of 0.02
 C30-H30
 1.909011 with sigma of 0.02
 Dy1-H30
 2.921321 with sigma of 0.02
3.a Riding coordinates:
 O34(H34), O48(H48)
3.b Ternary CH refined with riding coordinates:
 O3(H3), O7(H7)
3.c Me refined with riding coordinates:
 C2(H2A,H2B,H2C), C6(H6A,H6B,H6C), C1(H1A,H1B,H1C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C22(H22A,H22B,H22C), C13(H13A,H13B,H13C), C24(H24A,H24B,H24C),
 C34(H34A,H34B,H34C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C10(H10A,H10B,
 H10C), C8(H8A,H8B,H8C), C33(H33A,H33B,H33C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C26(H26A,H26B,H26C), C31(H31A,H31B,H31C), C28(H28A,H28B,H28C),
 C20(H20A,H20B,H20C)
3.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C32(H32A,H32B,H32C), C47(H47A,H47B,H47C), C49(H49A,H49B,
 H49C), C50(H50A,H50B,H50C)
3.e Idealised tetrahedral OH refined as rotating group:
 O49(H49), O50(H50)
;
_shelx_res_checksum              82829
_olex2_submission_special_instructions 'No special instructions were received'