Sodium and Potassium Ion Directed Self-Assembled Multinuclear Assembly of Divalent Nickel or Copper and l-Leucine Derived Ligand
Mrigendra Dubey; Rik Rani Koner; Manabendra Ray; Inorganic Chemistry 48 (2009) 9294–9302; doi:10.1021/ic9011444

data_4303274
_publ_contact_author_address
;Department of Chemistry
Indian Institute of Technology Guwahati
India 781039
;
_publ_contact_author_email       manabray@iitg.ernet.in
_publ_contact_author_name        'Dr. Manabendra Ray'
_publ_section_title
;
Sodium and Potassium Ion Directed Self-Assembled Multinuclear Assembly of
Divalent Nickel or Copper and l-Leucine Derived Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9294
_journal_page_last               9302
_journal_paper_doi               10.1021/ic9011444
_journal_volume                  48
_journal_year                    2009
_chemical_absolute_configuration syn
_chemical_compound_source        Synthesized
_chemical_formula_moiety         'C78 H108 Cu3 K N6 O18, N O4, 2(C O), 7(O)'
_chemical_formula_sum            'C80 H108 Cu3 K N7 O31'
_chemical_formula_weight         1893.45
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      20
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_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                   17.8717(16)
_cell_length_b                   21.262(2)
_cell_length_c                   26.901(3)
_cell_measurement_reflns_used    5064
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.79
_cell_measurement_theta_min      2.28
_cell_volume                     10222.1(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    WinGX
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            41985
_diffrn_reflns_theta_full        20.59
_diffrn_reflns_theta_max         20.59
_diffrn_reflns_theta_min         1.49
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_T_max  0.8673
_exptl_absorpt_correction_T_min  0.7582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Diamond
_exptl_crystal_F_000             3964
_exptl_crystal_recrystallization_method 'Methanol Acetonitrile'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_coef       0.00052(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         5180
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0546
_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^)+(0.1153P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1432
_refine_ls_wR_factor_ref         0.1485
_reflns_number_gt                4499
_reflns_number_total             5180
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic9011444_si_002_6.cif
_cod_data_source_block           Capsule_6
_cod_original_sg_symbol_Hall     'C 2c 2 '
_cod_database_code               4303274