Diastereoselective formation of a dicopper(i) helicate with a chiral tetradentate pyridylthiazole ligand.
Tsang, Chui-Shan; Yeung, Ho-Lun; Wong, Wing-Tak; Kwong, Hoi-Lun; Chemical communications (Cambridge, England) 34 (2009) 1999–2001; doi:10.1039/b900264b

data_7104316
_publ_section_title
;
 Diastereoselective formation of a dicopper(i) helicate with a chiral
 tetradentate pyridylthiazole ligand.
;
_journal_issue                   15
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1999
_journal_page_last               2001
_journal_paper_doi               10.1039/b900264b
_journal_volume                  34
_journal_year                    2009
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C60 H60 Cu2 N8 S4, 2(F6 P)'
_chemical_formula_sum            'C60 H60 Cu2 F12 N8 P2 S4'
_chemical_formula_weight         1438.42
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.410(3)
_cell_length_b                   22.331(4)
_cell_length_c                   11.2911(18)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.489
_cell_measurement_theta_min      22.451
_cell_volume                     4137.6(11)
_computing_cell_refinement       'SAINT v7.34A(Bruker, 2006)'
_computing_data_collection       'SMART (Bruker, 1996)'
_computing_data_reduction
'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2004)'
_computing_molecular_graphics    'ORTEP-II (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '\w & \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  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0856
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            28447
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.54
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.774713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
There existed large potential solvent void volume of about 660\%A^3^,
i.e. 1341.7\%A^3^ [32.4%] per unit cell. Attempts to locate the solvates
were not very successful, only one dichloromethane and one water solvates
could be located, as such a void volume of about 380\%A^3^ still remains.
As a result, the PLATON-SQUEEZE program was run and found that there may be
as much as 191 electron counts in the void. Due to the fact that the data
was colelcted at room temperature of 27\%C, the probability of finding all
the solvates which possibly were disordered is deemed to be low; the
solvent-free reflection data were then obtained from the SQUEEZE program
and used in subsequent SHELXL refinement until convergence.
PLATON was then run again with the new .hkl and .res files with the
instruction 'CALC FCF' to produce the final FoFc-CIF on .hkp, which was
then renamed to the .fcf file.
Thus this CIF only contain the major complex without any solvates located.
;
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details 'Flack (1983). 4118 Friedel pairs'
_refine_ls_abs_structure_Flack   0.008(9)
_refine_ls_extinction_coef       0.000266(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         9405
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0025P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0415
_refine_ls_wR_factor_ref         0.0438
_reflns_number_gt                4127
_reflns_number_total             9405
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b900264b.txt
_cod_data_source_block           shelxl
_cod_database_code               7104316