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_7048159
_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 H74 Co5 Gd4 N2 O44, 3(C H4 O)'
_chemical_formula_sum            'C41 H96 Co5 Gd4 N2 O47'
_chemical_formula_weight         2292.84
_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                 101.45(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.366(3)
_cell_length_b                   28.431(6)
_cell_length_c                   21.262(4)
_cell_measurement_reflns_used    13178
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      55.01
_cell_measurement_theta_min      6.04
_cell_volume                     7919(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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_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  0.0999
_diffrn_reflns_av_unetI/netI     0.0925
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            69224
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.019
_exptl_absorpt_coefficient_mu    4.412
_exptl_absorpt_correction_T_max  0.6667
_exptl_absorpt_correction_T_min  0.3511
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.923
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4492
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.500
_refine_diff_density_min         -2.773
_refine_diff_density_rms         0.226
_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     913
_refine_ls_number_reflns         17971
_refine_ls_number_restraints     1337
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0747
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0687P)^2^+107.8032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1927
_refine_ls_wR_factor_ref         0.2074
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13178
_reflns_number_total             17971
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04153a2.cif
_cod_data_source_block           2_Co5Gd4
_cod_depositor_comments
'Adding full bibliography for 7048154--7048159.cif.'
_cod_database_code               7048159
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.667
_shelx_estimated_absorpt_t_min   0.351
_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
 O30-C30
 1.47 with sigma of 0.01
 O45-C39
 1.35 with sigma of 0.01
 O46-C40
 1.35 with sigma of 0.01
 O47-C41
 1.35 with sigma of 0.01
 O27-C27'
 1.34 with sigma of 0.02
 O27-C27
 1.34 with sigma of 0.02
 O23-C23
 1.47 with sigma of 0.05
3. Rigid bond restraints
 O27, C27, C27'
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O31, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O30, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
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 O21 \\sim O22 \\sim O23 \\sim O24 \\sim O25
\\sim O26 \\sim O27 \\sim O28 \\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 \\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
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 C19 \\sim C20 \\sim C21 \\sim C22 \\sim C24 \\sim C25 \\sim C26
\\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34
\\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim
C27' \\sim C25' \\sim C23: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.05
5. Others
 Fixed Sof: C25(0.5) C27(0.5) C27'(0.5) C25'(0.5)
6.a Riding coordinates:
 O25(H25), O26(H26), O32(H32), O33(H33), O34(H34), O45(H45), O46(H46), O47(H47)
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), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C38(H38A,H38B,
 H38C)
6.c Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C)
;
_shelx_res_checksum              35692
_olex2_submission_special_instructions 'No special instructions were received'