Tetradecanuclearity in 3d-4f chemistry: relaxation and magnetocaloric effects in [NiLn] species.
Canaj, Angelos B.; Kalofolias, Dimitris A.; Siczek, Milosz; Lis, Tadeusz; McNab, Robbie; Lorusso, Giulia; Inglis, Ross; Evangelisti, Marco; Milios, Constantinos J.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 3449–3452; doi:10.1039/c7dt00102a

data_7041992
_publ_section_title
;
 Tetradecanuclearity in 3d-4f chemistry: relaxation and magnetocaloric
 effects in [NiLn] species.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3449
_journal_page_last               3452
_journal_paper_doi               10.1039/c7dt00102a
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety
'C152 H154 Dy8 N12 Ni6 O52, (C2 H3 N), 2(N O3), 0.5(H2 O)'
_chemical_formula_sum            'C154 H158 Dy8 N15 Ni6 O58.5'
_chemical_formula_weight         4807.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-12-02 deposited with the CCDC.
2017-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                69.78(4)
_cell_angle_beta                 83.79(3)
_cell_angle_gamma                84.34(3)
_cell_formula_units_Z            1
_cell_length_a                   14.200(5)
_cell_length_b                   18.006(7)
_cell_length_c                   18.029(7)
_cell_measurement_reflns_used    7862
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      25.663
_cell_measurement_theta_min      2.715
_cell_volume                     4291(3)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type
;
Xcalibur R kappa-geometry diffractometer with a Ruby CCD detector
;
_diffrn_measurement_method       w/
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.0928
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31346
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         25.663
_diffrn_reflns_theta_min         2.715
_exptl_absorpt_coefficient_mu    4.164
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_correction_T_min  0.455
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5
Analytical numeric absorption correction using a
multifaceted crystal model based on expressions
derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.860
_exptl_crystal_description       plate
_exptl_crystal_F_000             2351
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.958
_refine_diff_density_min         -1.057
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1117
_refine_ls_number_reflns         16022
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0848P)^2^+15.1043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1499
_refine_ls_wR_factor_ref         0.1897
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10025
_reflns_number_total             16022
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00102a2.cif
_cod_data_source_block           at2075a
_cod_depositor_comments
'Adding full bibliography for 7041992--7041993.cif.'
_cod_original_formula_sum        'C154 H158 Dy8 N15 Ni6 O58.50'
_cod_database_code               7041992
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.411
_shelx_estimated_absorpt_t_max   0.819
_shelx_res_checksum              9284