Metal clusters constructed by dihydrazide ligand: Synthesis, structure and magnetic properties
Dongcheng Liu; Zilu Chen; Wanyun Huang; Suni Qin; Liping Jiang; Suping Zhou; Fupei Liang; Inorganica Chimica Acta 400 (2013) 179–183; doi:

data_1516941
_publ_section_title
;
 Metal clusters constructed by dihydrazide ligand: Synthesis, structure
 and magnetic properties
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              179
_journal_page_last               183
_journal_volume                  400
_journal_year                    2013
_chemical_formula_moiety         C103H88Cu9N24O19,2(C3H7NO),2(C2H7N)
_chemical_formula_sum            'C113 H116 Cu9 N28 O21'
_chemical_formula_weight         2774.29
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   33.552(7)
_cell_length_b                   11.631(2)
_cell_length_c                   30.295(6)
_cell_measurement_reflns_used    34216
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      27.5742
_cell_measurement_theta_min      3.0689
_cell_volume                     11822(4)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_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  0.0785
_diffrn_reflns_av_sigmaI/netI    0.0871
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            70378
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.665
_exptl_absorpt_correction_T_max  0.7537
_exptl_absorpt_correction_T_min  0.6263
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5676
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.300
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.010(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1463
_refine_ls_number_reflns         20527
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0853
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1218P)^2^+34.6462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2231
_refine_ls_wR_factor_ref         0.2325
_reflns_number_gt                18514
_reflns_number_total             20527
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-400-179-183-1.cif
_cod_data_source_block           110
_cod_original_sg_symbol_H-M      Pca2(1)
_cod_database_code               1516941