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_4336954
_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         'C46 H58 N4 Ni4 O12, 2(C8 H7 O2), 4(H2 O)'
_chemical_formula_sum            'C62 H80 N4 Ni4 O20'
_chemical_formula_weight         1436.14
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 94.6647(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.02270(10)
_cell_length_b                   18.6158(3)
_cell_length_c                   16.4947(3)
_cell_measurement_reflns_used    24480
_cell_measurement_temperature    295
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.71
_cell_volume                     3373.44(9)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material
'SHELXL-97 (Sheldrick, 1997), PARST (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius Kappa 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  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24480
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    1.172
_exptl_absorpt_correction_T_max  0.614
_exptl_absorpt_correction_T_min  0.555
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SORTAV (R.H. Blessing, Acta Crystallogr., 1995, A51, 33)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.092(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         8234
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0800P)^2^+0.5808P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1217
_reflns_number_gt                7207
_reflns_number_total             8234
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic401337q_si_002_1.cif
_cod_data_source_block           3.4H2O
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4336954