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_7006576
_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 N8 S4 Pd2, 3(C3 H7 NO)'
_chemical_formula_sum            'C69 H97 N11 O3 Pd2 S4'
_chemical_formula_weight         1469.62
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 94.30(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   34.286(7)
_cell_length_b                   10.232(2)
_cell_length_c                   20.489(4)
_cell_measurement_temperature    120(2)
_cell_volume                     7168(2)
_computing_cell_refinement       'SAINT v.5.0 (Bruker AXS, 1997)'
_computing_data_collection       'SMART v.5.0 (Bruker AXS, 1997)'
_computing_data_reduction        'SAINT v.5.0 (Bruker AXS, 1997)'
_computing_molecular_graphics    'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material  'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_structure_solution    'SHELXTL v6.12 (Bruker AXS, 2001)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       'Thin slice \w 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  0.2114
_diffrn_reflns_av_sigmaI/netI    0.1319
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35855
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.671
_exptl_absorpt_correction_T_max  0.9867
_exptl_absorpt_correction_T_min  0.7614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v.2.03'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.02
_refine_diff_density_max         10.137
_refine_diff_density_min         -14.035
_refine_diff_density_rms         0.525
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.516
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         6324
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      2.514
_refine_ls_R_factor_all          0.2704
_refine_ls_R_factor_gt           0.2157
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4593
_refine_ls_wR_factor_ref         0.4756
_reflns_number_gt                3703
_reflns_number_total             6324
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b512068c.txt
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7006576