Self-sorting of equilibrating metallosupramolecular DCLs via constitutional crystallization.
Barboiu, Mihail; Dumitru, Florina; Legrand, Yves-Marie; Petit, Eddy; van der Lee, Arie; Chemical communications (Cambridge, England) 34 (2009) 2192–2194; doi:10.1039/b900155g

data_7104333
_publ_section_title
;
 Self-sorting of equilibrating metallosupramolecular DCLs via
 constitutional crystallization.
;
_journal_issue                   16
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2192
_journal_page_last               2194
_journal_paper_doi               10.1039/b900155g
_journal_volume                  34
_journal_year                    2009
_chemical_formula_moiety         '2(C22 H20 F3 N4 O6 S Zn), 2(C F3 O3 S)'
_chemical_formula_sum            'C46 H40 F12 N8 O18 S4 Zn2'
_chemical_formula_weight         1479.87
_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
_cell_angle_alpha                81.785(3)
_cell_angle_beta                 89.709(3)
_cell_angle_gamma                87.927(3)
_cell_formula_units_Z            2
_cell_length_a                   8.9330(3)
_cell_length_b                   10.5894(4)
_cell_length_c                   30.0903(10)
_cell_measurement_reflns_used    8107
_cell_measurement_temperature    173
_cell_measurement_theta_max      33.6074
_cell_measurement_theta_min      3.6799
_cell_volume                     2815.34(17)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 16.0143
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_details
;
1 omega 27.47 100.47 1.0000 5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 32.0000 -140.0000 -40.0000 0.0000 0.0000 73

2 omega 2.00 103.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 32.0000 70.0000 -140.0000 0.0000 0.0000 101

3 omega -83.69 -5.69 1.0000 5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -32.0000 110.0000 -290.0000 0.0000 0.0000 78

4 phi -180.00 170.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
0.0000 32.0000 0.0000 - 0.0000 0.0000 350

5 omega 2.00 103.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 32.0000 70.0000 -20.0000 0.0000 0.0000 101

6 omega 2.00 103.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 32.0000 70.0000 -270.0000 0.0000 0.0000 101

;
_diffrn_measurement_device       'Oxford Diffraction XCALIBUR'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      -0.0538779135
_diffrn_orient_matrix_UB_12      -0.0234299333
_diffrn_orient_matrix_UB_13      -0.0136635994
_diffrn_orient_matrix_UB_21      0.0049740005
_diffrn_orient_matrix_UB_22      -0.0602581653
_diffrn_orient_matrix_UB_23      0.0136952337
_diffrn_orient_matrix_UB_31      -0.0580543030
_diffrn_orient_matrix_UB_32      0.0198967321
_diffrn_orient_matrix_UB_33      0.0138547070
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.070
_diffrn_reflns_av_sigmaI/netI    0.087
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            58657
_diffrn_reflns_theta_full        30.635
_diffrn_reflns_theta_max         33.665
_diffrn_reflns_theta_min         3.686
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.120
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.20
_refine_diff_density_min         -2.13
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8913
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         7062
_refine_ls_number_restraints     1036
_refine_ls_R_factor_all          0.1635
_refine_ls_R_factor_gt           0.0689
_refine_ls_shift/su_max          0.000535
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
15.3 -7.15 8.18
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1253
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0738
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              16
_reflns_limit_k_min              -15
_reflns_limit_l_max              46
_reflns_limit_l_min              0
_reflns_number_gt                7062
_reflns_number_total             20555
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0689
_oxford_refine_ls_scale          2.150(3)
_oxford_reflns_number_all        20555
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            b900155g.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7104333