A series of hetero-multi-spin Ln2Cu3 complexes based on a methyl-pyrazole nitronyl nitroxide radical with slow magnetic relaxation behaviors
Tian, Li; Liu, Zhong Yi; Shi, Jian Yun; Chen, Pengyun; Wu, Mingze; Dalton Transactions  (2019) –; doi:10.1039/C9DT00981G

data_7700072
_publ_section_title
;
 A series of hetero-multi-spin Ln2Cu3 complexes based on a methyl-pyrazole
 nitronyl nitroxide radical with slow magnetic relaxation behaviors
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT00981G
_journal_year                    2019
_chemical_formula_sum            'C61.8 H48.1 I4 N7.5 O8.7 Zn2'
_chemical_formula_weight         1673.31
_chemical_melting_point          617.7
_chemical_name_systematic
'bis-bis(isoquinolin-5-yl)-isophthalate-tetraiodo-di-zinc(ii) acetonitrile solvate solvate solvate tetrahydrofuran solvate solvate solvate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           59
_space_group_name_Hall           '-P 2ab 2a'
_space_group_name_H-M_alt        'P m m n'
_symmetry_space_group_name_Hall  '-P 2ab 2a'
_symmetry_space_group_name_H-M   'P m m n :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-05-13 deposited with the CCDC.    2019-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.865(4)
_cell_length_b                   24.913(5)
_cell_length_c                   7.4000(15)
_cell_measurement_reflns_used    90887
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      33.548
_cell_measurement_theta_min      0.361
_cell_volume                     3293.5(12)
_computing_cell_refinement       HKL3000sm
_computing_data_collection       'PAL BL2D-SMDC Program'
_computing_data_reduction        HKL3000sm
_computing_structure_refinement  SHELXL
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.630
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            27994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        22.210
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         2.021
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    1.904
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.851
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL3000sm Scalepack'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_description       block
_exptl_crystal_F_000             1626
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH3CN, C4H8O'
_exptl_crystal_size_max          0.112
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.322
_refine_diff_density_min         -2.679
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4357
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0876P)^2^+4.9180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1315
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4288
_reflns_number_total             4357
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00981g2.cif
_cod_data_source_block           MeCN
_cod_original_cell_volume        3293.5(11)
_cod_original_formula_sum        'C61.80 H48.10 I4 N7.50 O8.70 Zn2'
_cod_database_code               7700072
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.815
_shelx_estimated_absorpt_t_max   0.832
_shelx_res_checksum              43652
_shelx_hkl_checksum              81564