An Unprecedented Octadecanuclear Copper(II) Pyrazolate-Phosphonate Nanocage: Synthetic, Structural, Magnetic, and Mechanistic Study
Javeed Ahmad Sheikh; Himanshu Sekhar Jena; Amit Adhikary; Sajal Khatua; Sanjit Konar; Inorganic Chemistry 52 (2013) 9717–9719; doi:10.1021/ic401754q

data_4335928
_publ_section_title
;
 An Unprecedented Octadecanuclear Copper(II) Pyrazolate-Phosphonate
 Nanocage: Synthetic, Structural, Magnetic, and Mechanistic Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9717
_journal_page_last               9719
_journal_paper_doi               10.1021/ic401754q
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C24 H25 Cu3 N11 O7'
_chemical_formula_sum            'C24 H25 Cu3 N11 O7'
_chemical_formula_weight         770.20
_space_group_IT_number           34
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 -2n'
_symmetry_space_group_name_H-M   'P n n 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.180(10)
_cell_length_b                   23.340(16)
_cell_length_c                   10.729(7)
_cell_measurement_reflns_used    5846
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.24
_cell_measurement_theta_min      2.38
_cell_volume                     3551(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0600
_diffrn_reflns_av_sigmaI/netI    0.0729
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            20480
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    1.833
_exptl_absorpt_correction_T_max  0.632
_exptl_absorpt_correction_T_min  0.438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       Block
_exptl_crystal_F_000             1556
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.655
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.12(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         5976
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0644
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1330P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1921
_refine_ls_wR_factor_ref         0.2129
_reflns_number_gt                3978
_reflns_number_total             6328
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401754q_si_002.cif
_cod_data_source_block           936434
_cod_database_code               4335928