Self-Assembled Tetra- and Pentanuclear Nickel(II) Aggregates From Phenoxido-Based Ligand -Bound {Ni2} Fragments: Carboxylate Bridge Controlled Structures
Aloke Kumar Ghosh; Michael Shatruk; Valerio Bertolasi; Kausikisankar Pramanik; Debashis Ray; Inorganic Chemistry 52 (2013) 13894–13903; doi:10.1021/ic401337q

data_4336955
_publ_contact_author_address
; Prof. Debashis Ray 
 Department of Chemistry 
 Indian Institute of Technology
 Kharagpur-721302
 India 
;
_publ_contact_author_email       dray@chem.iitkgp.ernet.in
_publ_contact_author_fax         03222-255303
_publ_contact_author_name        'Prof. Debashis Ray'
_publ_contact_author_phone       03222-283324
_publ_section_title
;
 Self-Assembled Tetra- and Pentanuclear Nickel(II) Aggregates From
 Phenoxido-Based Ligand -Bound {Ni2} Fragments: Carboxylate Bridge
 Controlled Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13894
_journal_page_last               13903
_journal_paper_doi               10.1021/ic401337q
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C48 H74 N4 Ni5 O20, 4(C3 H7 N O), 2(H2 O)'
_chemical_formula_sum            'C60 H106 N8 Ni5 O26'
_chemical_formula_weight         1649.08
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 90.9944(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.8638(8)
_cell_length_b                   16.5597(11)
_cell_length_c                   19.4940(14)
_cell_measurement_reflns_used    49815
_cell_measurement_temperature    295
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      1.61
_cell_volume                     3829.2(5)
_computing_cell_refinement       Brucker
_computing_data_collection       Brucker
_computing_data_reduction        Brucker
_computing_molecular_graphics    'ORTEP III (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Brucker-APEX-2 CCD'
_diffrn_measurement_method       '\f scans 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  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            49815
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    1.285
_exptl_absorpt_correction_T_max  0.738
_exptl_absorpt_correction_T_min  0.630
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_description       block
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         8295
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0760P)^2^+3.9089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1455
_reflns_number_gt                5903
_reflns_number_total             8295
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic401337q_si_002_2.cif
_cod_data_source_block           1.2H2O.4DMF
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4336955