Lanthanide-Directed Fabrication of Four Tetranuclear Quadruple Stranded Helicates Showing Magnetic Refrigeration and Slow Magnetic Relaxation.
Mondal, Amit Kumar; Jena, Himanshu Sekhar; Malviya, Amita; Konar, Sanjit; Inorganic chemistry 55 (2016) 5237–5244; doi:10.1021/acs.inorgchem.6b00177

data_4347454
_publ_section_title
;
 Lanthanide-Directed Fabrication of Four Tetranuclear Quadruple Stranded
 Helicates Showing Magnetic Refrigeration and Slow Magnetic Relaxation.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5237
_journal_page_last               5244
_journal_paper_doi               10.1021/acs.inorgchem.6b00177
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C88 H97 Er4 N16 O26, 2(N O3), 9(O H2)'
_chemical_formula_sum            'C88 H115 Er4 N18 O41'
_chemical_formula_weight         2731.88
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                69.904(5)
_cell_angle_beta                 81.134(5)
_cell_angle_gamma                77.908(5)
_cell_formula_units_Z            2
_cell_length_a                   13.205(3)
_cell_length_b                   17.931(4)
_cell_length_c                   24.533(5)
_cell_measurement_reflns_used    9877
_cell_measurement_temperature    104(2)
_cell_measurement_theta_max      25.81
_cell_measurement_theta_min      2.27
_cell_volume                     5313(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      104(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0904
_diffrn_reflns_av_unetI/netI     0.0951
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            25065
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.809
_diffrn_reflns_theta_min         2.161
_exptl_absorpt_coefficient_mu    3.221
_exptl_absorpt_correction_T_max  0.447
_exptl_absorpt_correction_T_min  0.279
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_description       block
_exptl_crystal_F_000             2702
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.370
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.287
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1179
_refine_ls_number_reflns         20445
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.1082
_refine_ls_R_factor_gt           0.0690
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.8161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1767
_refine_ls_wR_factor_ref         0.1957
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18742
_reflns_number_total             20445
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00177_si_002.cif
_cod_data_source_block           3
_cod_original_cell_volume        5312.8(19)
_cod_database_code               4347454
_shelxl_version_number           2013-4
_shelx_res_checksum              95126
_shelx_hkl_checksum              31682