Controlled formation and topologies of thiophenolate-based macrocycles: rings, cylinders and bowls.
Christensen, Aase; Mayer, Christoph; Jensen, Frank; Bond, Andrew D.; McKenzie, Christine J.; Dalton transactions (Cambridge, England : 2003)  (2006) 108–120; doi:10.1039/b512068c

data_7006577
_publ_section_title
;
 Controlled formation and topologies of thiophenolate-based
 macrocycles: rings, cylinders and bowls.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              108
_journal_page_last               120
_journal_paper_doi               10.1039/b512068c
_journal_year                    2006
_chemical_formula_moiety         'C60 H76 N12 O12 S4 Zn4, 5(C2 H3 N)'
_chemical_formula_sum            'C70 H91 N17 O12 S4 Zn4'
_chemical_formula_weight         1752.32
_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
_cell_angle_alpha                107.850(3)
_cell_angle_beta                 103.482(3)
_cell_angle_gamma                102.425(3)
_cell_formula_units_Z            4
_cell_length_a                   15.567(2)
_cell_length_b                   22.548(3)
_cell_length_c                   26.568(3)
_cell_measurement_reflns_used    4957
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      15.79
_cell_measurement_theta_min      2.30
_cell_volume                     8207.7(18)
_computing_cell_refinement       'SAINT v.7.06a (Bruker, 2003)'
_computing_data_collection       'APEX2 v.1.0-8 (Bruker-Nonius, 2003)'
_computing_data_reduction        'SAINT v.7.06a (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL v.6.10 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL v.6.10 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXTL v.6.10 (Sheldrick, 2000)'
_computing_structure_solution    'SHELXTL v.6.10 (Sheldrick, 2000)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.812
_diffrn_measurement_device_type  'Bruker-Nonius X8APEX-II CCD'
_diffrn_measurement_method       'thin-slice \w and \f 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  0.1485
_diffrn_reflns_av_sigmaI/netI    0.2144
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            65820
_diffrn_reflns_theta_full        20.82
_diffrn_reflns_theta_max         22.25
_diffrn_reflns_theta_min         3.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.323
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v.2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3640
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.493
_refine_diff_density_min         -1.103
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     984
_refine_ls_number_reflns         16884
_refine_ls_number_restraints     323
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.2123
_refine_ls_R_factor_gt           0.1007
_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^)+(0.1505P)^2^+23.2301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2526
_refine_ls_wR_factor_ref         0.3139
_reflns_number_gt                7972
_reflns_number_total             16884
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b512068c.txt
_cod_data_source_block           6
_cod_database_code               7006577