Preparation of Site-Differentiated Mixed Ligand and Mixed Ligand/Mixed Metal Metallacrowns
George Psomas; Ann J. Stemmler; Catherine Dendrinou-Samara; Jeffrey J. Bodwin; Manuela Schneider; Maria Alexiou; Jeff W. Kampf; Dimitris P. Kessissoglou; Vincent L. Pecoraro; Inorganic Chemistry 40 (2001) 1562–1570; doi:10.1021/ic000578+

data_4327550
_publ_section_title
;
 Preparation of Site-Differentiated Mixed Ligand and Mixed Ligand/Mixed
 Metal Metallacrowns
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1562
_journal_page_last               1570
_journal_paper_doi               10.1021/ic000578+
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C46 H48 N12 Ni4 O12 S2'
_chemical_formula_weight         1259.92
_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                87.5160(10)
_cell_angle_beta                 82.6380(10)
_cell_angle_gamma                71.4650(10)
_cell_formula_units_Z            2
_cell_length_a                   11.1909(2)
_cell_length_b                   13.6377(2)
_cell_length_c                   17.7623(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      26.47
_cell_measurement_theta_min      2.37
_cell_volume                     2549.04(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      158(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36828
_diffrn_reflns_theta_full        26.47
_diffrn_reflns_theta_max         26.47
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    1.611
_exptl_absorpt_correction_T_max  ?0.879
_exptl_absorpt_correction_T_min  0.760
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.139
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.0007(2)
_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   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     710
_refine_ls_number_reflns         10429
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.079
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+5.6511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1021
_reflns_number_gt                8555
_reflns_number_total             10429
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0005782B_1.cif
_cod_data_source_block           IC000578-1A
_cod_database_code               4327550