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_4347452
_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 H98 Gd4 N16 O26, 2(C2 H3 O2), 4(O H2)'
_chemical_formula_sum            'C92 H112 Gd4 N16 O34'
_chemical_formula_weight         2606.92
_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                108.258(5)
_cell_angle_beta                 94.285(5)
_cell_angle_gamma                90.647(5)
_cell_formula_units_Z            2
_cell_length_a                   17.336(3)
_cell_length_b                   17.945(3)
_cell_length_c                   18.528(3)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    106(2)
_cell_measurement_theta_max      26.21
_cell_measurement_theta_min      2.31
_cell_volume                     5454.8(16)
_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-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      106(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0627
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            232351
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.256
_diffrn_reflns_theta_min         2.253
_exptl_absorpt_coefficient_mu    2.484
_exptl_absorpt_correction_T_max  0.537
_exptl_absorpt_correction_T_min  0.366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_description       block
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;
 ?
;
_refine_diff_density_max         0.873
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.233
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1271
_refine_ls_number_reflns         21990
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.233
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0898
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0213P)^2^+1.7621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2054
_refine_ls_wR_factor_ref         0.2144
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18535
_reflns_number_total             21990
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00177_si_002.cif
_cod_data_source_block           1
_cod_database_code               4347452
_shelxl_version_number           2013-4
_shelx_res_checksum              62358
_shelx_hkl_checksum              41495