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_7048156
_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         'C37 H74 Eu4 N2 Ni5 O44, 3(C H4 O)'
_chemical_formula_sum            'C40 H40 Eu4 N2 Ni5 O50'
_chemical_formula_weight         2250.13
_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
_atom_sites_solution_primary     iterative
_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                 101.85(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.335(3)
_cell_length_b                   28.284(6)
_cell_length_c                   21.178(4)
_cell_measurement_reflns_used    11387
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      54.92
_cell_measurement_theta_min      6.07
_cell_volume                     7817(3)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.967
_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  0.0908
_diffrn_reflns_av_unetI/netI     0.0727
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            60142
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         3.035
_exptl_absorpt_coefficient_mu    4.431
_exptl_absorpt_correction_T_max  0.642
_exptl_absorpt_correction_T_min  0.221
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.912
_exptl_crystal_description       block
_exptl_crystal_F_000             4344
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.380
_refine_diff_density_min         -1.735
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     885
_refine_ls_number_reflns         14875
_refine_ls_number_restraints     1335
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0747
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0836P)^2^+111.1545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1816
_refine_ls_wR_factor_ref         0.1943
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11387
_reflns_number_total             14875
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04153a2.cif
_cod_data_source_block           4_Ni5Eu4
_cod_depositor_comments
'Adding full bibliography for 7048154--7048159.cif.'
_cod_original_cell_volume        7818(3)
_cod_database_code               7048156
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.666
_shelx_estimated_absorpt_t_min   0.270
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O33-H33
 0.85 with sigma of 0.01
 O36-H36
 0.85 with sigma of 0.01
 O6-C6
 1.65 with sigma of 0.02
 C33-H33
 1.914091 with sigma of 0.02
 Eu3-H33
 2.891828 with sigma of 0.02
 C36-H36
 1.873283 with sigma of 0.02
 Eu2-H36
 2.936939 with sigma of 0.02
3. Rigid bond restraints
 C3, O3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O33, C33
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O7 \\sim O1 \\sim O8 \\sim O5 \\sim O4 \\sim O3 \\sim O6 \\sim O2 \\sim O16
\\sim O21 \\sim O23 \\sim O20 \\sim O15 \\sim O24 \\sim O13 \\sim O31 \\sim O19
\\sim O32 \\sim O14 \\sim O11 \\sim O22 \\sim O18 \\sim O12 \\sim O9 \\sim O17
\\sim O36 \\sim O27 \\sim O35 \\sim O38 \\sim O10 \\sim O33 \\sim O26 \\sim O29
\\sim O25 \\sim O28 \\sim O37 \\sim O39 \\sim O42 \\sim O30 \\sim O43 \\sim O40
\\sim O34 \\sim O44 \\sim O41 \\sim O45 \\sim O46 \\sim O47: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.02
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C19 \\sim C31 \\sim C15 \\sim C23 \\sim C1 \\sim C11 \\sim C21 \\sim C32 \\sim
C13 \\sim C7 \\sim C2 \\sim C8 \\sim C29 \\sim C4 \\sim C17 \\sim C10 \\sim C25
\\sim C5 \\sim C24 \\sim C12 \\sim C36 \\sim C16 \\sim C27 \\sim C14 \\sim C9
\\sim C22 \\sim C30 \\sim C3 \\sim C35 \\sim C20 \\sim C37 \\sim C28 \\sim C38
\\sim C18 \\sim C46 \\sim C45 \\sim C33 \\sim C26 \\sim C47 \\sim C6: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.05
Uanis(O6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.05
5.a Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C32(H32A,H32B,H32C), C7(H7A,H7B,H7C), C2(H2A,H2B,H2C),
 C8(H8A,H8B,H8C), C4(H4A,H4B,H4C), C10(H10A,H10B,H10C), C5(H5A,H5B,H5C),
 C24(H24A,H24B,H24C), C12(H12A,H12B,H12C), C36(H36A,H36B,H36C), C16(H16A,H16B,
 H16C), C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C30(H30A,H30B,H30C), C3(H3A,
 H3B,H3C), C35(H35A,H35B,H35C), C20(H20A,H20B,H20C), C37(H37A,H37B,H37C),
 C28(H28A,H28B,H28C), C38(H38A,H38B,H38C), C18(H18A,H18B,H18C), C33(H33A,H33B,
 H33C), C26(H26A,H26B,H26C)
5.b Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C)
5.c Idealised tetrahedral OH refined as rotating group:
 O45(H45), O46(H46), O47(H47)
;
_shelx_res_checksum              92234
_olex2_submission_special_instructions 'No special instructions were received'