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_7006574
_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
;
C30 H38 N4 Ni2 S2 2+, 2(Cl O4 -), 0.5(C3 H7 N O), 0.5(C H4 O)
;
_chemical_formula_sum            'C32 H43.5 Cl2 N4.5 Ni2 O9 S2'
_chemical_formula_weight         887.65
_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                102.565(4)
_cell_angle_beta                 100.972(4)
_cell_angle_gamma                117.638(4)
_cell_formula_units_Z            2
_cell_length_a                   12.373(2)
_cell_length_b                   13.331(2)
_cell_length_c                   15.212(3)
_cell_measurement_reflns_used    5140
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.64
_cell_measurement_theta_min      2.72
_cell_volume                     2042.8(6)
_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      180(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0590
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17012
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.208
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Sheldrick, 2003)
Ratio of minimum to maximum apparent transmission: 0.551574
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             922
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.100
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         7118
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0760
_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^)+(0.1443P)^2^+4.8208P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2101
_refine_ls_wR_factor_ref         0.2342
_reflns_number_gt                5053
_reflns_number_total             7118
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b512068c.txt
_cod_data_source_block           3
_cod_original_formula_sum        'C32 H43.50 Cl2 N4.50 Ni2 O9 S2'
_cod_database_code               7006574