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

data_7001620
_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            'C44 H76 N6 O4 S2'
_chemical_formula_weight         817.23
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 91.98(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.449(2)
_cell_length_b                   19.417(3)
_cell_length_c                   18.976(2)
_cell_measurement_temperature    180(2)
_cell_volume                     4584.2(11)
_computing_cell_refinement       'STOE X-Area'
_computing_data_collection       'STOE X-Area'
_computing_data_reduction        'STOE X-Area'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       hemisphere
_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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19229
_diffrn_reflns_theta_full        29.29
_diffrn_reflns_theta_max         29.29
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_T_max  0.9682
_exptl_absorpt_correction_T_min  0.9528
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         6174
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0727P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1172
_reflns_number_gt                4497
_reflns_number_total             6174
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b908553j.txt
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7001620