Novel topological supramolecular architectures based on partially protonated butane-1,2,3,4-tetracarboxylato complexes: Synthesis, structures and magnetic properties
Hong-Lin Zhu; Jin-Li Qi; Jian-Li Lin; Wei Xu; Jiang Wu; Yue-Qing Zheng; Inorganica Chimica Acta 404 (2013) 49–57; doi:

data_1517702
_publ_section_title
;
 Novel topological supramolecular architectures based on partially
 protonated butane-1,2,3,4-tetracarboxylato complexes: Synthesis,
 structures and magnetic properties
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              49
_journal_page_last               57
_journal_volume                  404
_journal_year                    2013
_chemical_formula_moiety         'C72 H70 N8 Ni2 O30'
_chemical_formula_sum            'C72 H70 N8 Ni2 O30'
_chemical_formula_weight         1644.75
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                80.83(3)
_cell_angle_beta                 79.02(3)
_cell_angle_gamma                87.53(3)
_cell_formula_units_Z            1
_cell_length_a                   10.793(2)
_cell_length_b                   12.864(3)
_cell_length_c                   13.536(3)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.02
_cell_volume                     1821.2(7)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_sigmaI/netI    0.0756
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18089
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.02
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             854
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.352
_refine_diff_density_min         -1.910
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       0.0163(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         8247
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.1573
_refine_ls_R_factor_gt           0.0660
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0682P)^2^+5.3054P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1502
_refine_ls_wR_factor_ref         0.2400
_reflns_number_gt                4223
_reflns_number_total             8247
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-404-49-57-1.cif
_cod_data_source_block           shx97-1
_cod_original_cell_volume        1821.2(6)
_cod_database_code               1517702