The first binucleating amino-thiophenolate macrocycles with pendant hydroxyethyl groups
Gressenbuch, Mathias; Kersting, Berthold; Dalton Transactions  (2009) 5281–5283; doi:10.1039/b908553j

data_7001621
_publ_section_title
;
 The first binucleating amino-thiophenolate macrocycles with pendant
 hydroxyethyl groups
;
_journal_issue                   27
_journal_name_full               'Dalton Transactions'
_journal_page_first              5281
_journal_page_last               5283
_journal_paper_doi               10.1039/b908553j
_journal_year                    2009
_chemical_formula_sum            'C96 H176 N12 Na4 Ni2 O22 S4'
_chemical_formula_weight         2188.10
_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                67.639(10)
_cell_angle_beta                 71.354(12)
_cell_angle_gamma                71.855(12)
_cell_formula_units_Z            1
_cell_length_a                   12.049(2)
_cell_length_b                   17.177(2)
_cell_length_c                   17.654(2)
_cell_measurement_temperature    180(2)
_cell_volume                     3125.7(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_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  0.0848
_diffrn_reflns_av_sigmaI/netI    0.1266
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23060
_diffrn_reflns_theta_full        25.53
_diffrn_reflns_theta_max         25.53
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.445
_exptl_absorpt_correction_T_max  0.9363
_exptl_absorpt_correction_T_min  0.8970
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.013
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         10719
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_gt           0.0676
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0981P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1779
_refine_ls_wR_factor_ref         0.1951
_reflns_number_gt                5665
_reflns_number_total             10719
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b908553j.txt
_cod_data_source_block           7
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7001621