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_4335927
_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
'C112 H122 Cu18 N28 O34 P8, 4(C2 H3 N), 4(O) '
_chemical_formula_sum            'C120 H134 Cu18 N32 O38 P8'
_chemical_formula_weight         4024.26
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.566(4)
_cell_angle_beta                 68.987(4)
_cell_angle_gamma                82.835(4)
_cell_formula_units_Z            1
_cell_length_a                   15.165(3)
_cell_length_b                   16.196(2)
_cell_length_c                   18.978(3)
_cell_measurement_reflns_used    9653
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      25.91
_cell_measurement_theta_min      2.31
_cell_volume                     4210.7(12)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_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  0.0654
_diffrn_reflns_av_sigmaI/netI    0.0794
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37936
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    2.371
_exptl_absorpt_correction_T_max  0.515
_exptl_absorpt_correction_T_min  0.395
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_description       block
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.687
_refine_diff_density_min         -2.175
_refine_diff_density_rms         0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     980
_refine_ls_number_reflns         16491
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0666
_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^)+(0.1583P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1900
_refine_ls_wR_factor_ref         0.2504
_reflns_number_gt                14450
_reflns_number_total             16491
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401754q_si_001.cif
_cod_data_source_block           935277
_cod_database_code               4335927