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_7104334
_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_absolute_configuration ad
_chemical_formula_moiety         'C21 H15 F6 N3 O8 Pb S2'
_chemical_formula_sum            'C21 H15 F6 N3 O8 Pb S2'
_chemical_formula_weight         822.70
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   15.8406(5)
_cell_length_b                   16.1462(4)
_cell_length_c                   40.5039(14)
_cell_measurement_reflns_used    13820
_cell_measurement_temperature    173
_cell_measurement_theta_max      29.0416
_cell_measurement_theta_min      3.7328
_cell_volume                     10359.5(5)
_computing_cell_refinement
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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
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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
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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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 16.0143
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_details
;
1 omega -12.00 40.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 17.8630 77.0000 90.0000 0.0000 0.0000 52

2 omega -52.00 0.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 17.8630 -77.0000 270.0000 0.0000 0.0000 52

3 omega -53.00 -4.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 17.8630 -45.0000 330.0000 0.0000 0.0000 49

4 omega -53.00 -4.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 17.8630 -45.0000 210.0000 0.0000 0.0000 49

5 omega -53.00 -4.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 17.8630 -45.0000 120.0000 0.0000 0.0000 49

6 omega -12.00 40.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 17.8630 77.0000 180.0000 0.0000 0.0000 52

7 omega 40.00 89.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 17.8630 45.0000 60.0000 0.0000 0.0000 49

8 omega 40.00 89.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 17.8630 45.0000 210.0000 0.0000 0.0000 49

;
_diffrn_measurement_device       'Oxford Diffraction XCALIBUR'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      0.0175822520
_diffrn_orient_matrix_UB_12      0.0141244469
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_diffrn_orient_matrix_UB_21      0.0124856226
_diffrn_orient_matrix_UB_22      -0.0410235507
_diffrn_orient_matrix_UB_23      -0.0038768805
_diffrn_orient_matrix_UB_31      -0.0391939368
_diffrn_orient_matrix_UB_32      -0.0067307707
_diffrn_orient_matrix_UB_33      -0.0079937735
_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  0.026
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
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_diffrn_reflns_limit_k_min       -20
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_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            20575
_diffrn_reflns_theta_full        25.917
_diffrn_reflns_theta_max         29.120
_diffrn_reflns_theta_min         3.742
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.771
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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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            orange-red
_exptl_crystal_density_diffrn    2.111
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6304.0
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.51
_refine_diff_density_min         -1.32
_refine_ls_abs_structure_details 'Flack (1983), 2749 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.502(4)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         5996
_refine_ls_number_restraints     452
_refine_ls_R_factor_all          0.0386
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_refine_ls_shift/su_max          0.001483
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 0.00P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
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_reflns_limit_h_max              21
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_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              54
_reflns_limit_l_min              -53
_reflns_number_gt                4703
_reflns_number_total             5996
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.39
_oxford_diffrn_Wilson_scale      0.85
_oxford_refine_ls_r_factor_ref   0.0386
_oxford_refine_ls_scale          0.33612(12)
_oxford_reflns_number_all        5996
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            b900155g.txt
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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_H-M      'F d d 2 '
_cod_database_code               7104334