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_7048155
_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
'C38 H84 Co5 Eu4 N2 O44, 3(C H4 O), 0.75(C H3 O)'
_chemical_formula_sum            'C41.75 H99 Co5 Eu4 N2 O47.75'
_chemical_formula_weight         2295.71
_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                 100.866(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3061(3)
_cell_length_b                   28.4606(8)
_cell_length_c                   21.2498(8)
_cell_measurement_reflns_used    9528
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.0586
_cell_measurement_theta_min      2.7182
_cell_volume                     7903.0(4)
_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(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_av_unetI/netI     0.0948
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40507
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.724
_exptl_absorpt_coefficient_mu    4.241
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83874
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.929
_exptl_crystal_description       block
_exptl_crystal_F_000             4530
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.167
_refine_diff_density_min         -2.992
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     904
_refine_ls_number_reflns         15509
_refine_ls_number_restraints     1882
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.1270
_refine_ls_R_factor_gt           0.0927
_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^)+(0.0380P)^2^+184.8781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1759
_refine_ls_wR_factor_ref         0.1914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11270
_reflns_number_total             15509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04153a2.cif
_cod_data_source_block           1_Co5Eu4
_cod_depositor_comments
'Adding full bibliography for 7048154--7048159.cif.'
_cod_database_code               7048155
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.676
_shelx_estimated_absorpt_t_min   0.282
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C32-O32
 1.44 with sigma of 0.01
 C33-O33
 1.44 with sigma of 0.01
 C39-O39
 1.44 with sigma of 0.01
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O33, C33, Co3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C29
\\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C33' \\sim C34 \\sim C35 \\sim
C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim
C44 \\sim C45 \\sim C46: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8 \\sim O9
\\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim O16 \\sim O17
\\sim O18 \\sim O19 \\sim O20 \\sim O47 \\sim O21 \\sim O22 \\sim O23 \\sim O24
\\sim O25 \\sim O26 \\sim O27 \\sim O28 \\sim O48 \\sim O29 \\sim O30 \\sim O31
\\sim O32 \\sim O33 \\sim O34 \\sim O35 \\sim O36 \\sim O37 \\sim O38 \\sim O39
\\sim O40 \\sim O41 \\sim O42 \\sim O43 \\sim O44 \\sim O45 \\sim O46: 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
Uanis(C39) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O38) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C32) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Fixed Sof: C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5) C33'(0.5) H33D(0.5)
 H33E(0.5) H33F(0.5) O44(0.75) C44(0.75) H44A(0.75) H44B(0.75) H44C(0.75)
6.a Riding coordinates:
 O33(H33), O34(H34), O35(H35), O40(H40), O41(H41), O42(H42), O43(H43),
 O45(H45), O46(H46)
6.b Me refined with riding coordinates:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C),
 C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C26(H26A,H26B,
 H26C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33'(H33D,H33E,H33F), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C)
6.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,
 H45C), C46(H46A,H46B,H46C)
;
_shelx_res_checksum              76472
_olex2_submission_special_instructions 'No special instructions were received'