Valence-induced assembly of Cu(I)-Cu(II) ions into different discrete coordination architectures by a disk-shaped polypyridyl ligand.
Zhao, Qiang; Liu, Xiu-Ming; Song, Wei-Chao; Bu, Xian-He; Dalton transactions (Cambridge, England : 2003) 41 (2012) 6683–6688; doi:10.1039/c2dt00002d

data_7019048
_publ_section_title
;
 Valence-induced assembly of Cu(I)-Cu(II) ions into different discrete
 coordination architectures by a disk-shaped polypyridyl ligand.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6683
_journal_page_last               6688
_journal_paper_doi               10.1039/c2dt00002d
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C94.4 H58.4 Cl31.2 Cu6 I6 N24'
_chemical_formula_weight         3777.66
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   20.799(4)
_cell_length_b                   20.799(4)
_cell_length_c                   47.180(5)
_cell_measurement_reflns_used    22143
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1.2
_cell_volume                     17676(5)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)'
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'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       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  0.0496
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            41085
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    3.325
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.665
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            dark-blue
_exptl_crystal_density_diffrn    1.968
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             10008
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;In order to subtract the contribution from the disordered solvent molecules, the SQUEEZE command was applied, which gave a new HKL file. The number of located electrons is 3635, is included in the formula, formula weight, calculated density, and F(000). These residual electron density were assigned to 10.4 chloroform molecules. So SQUEEZE 10.4 chloroform molecules per formula unit. This value calculated based upon electrons analysis. (One chloroform molecules would give 58 e). So the tentative formula for this compound is presented as in the text.
See refs. (a) O. V. Dolomanov, D. B. Cordes, N. R. Champness, A. J. Blake, L. R. Hanton, G. B. Jameson, M. Schroder and C. Wilson. Chem. Commun., 2004, 642; (b) Y. Du, A. L. Thompson and D. O. Hare.Chem. Commun. 2008, 5987; (c) Y. F. Bi, X. T. Wang, W. P. Liao, X. F. Wang, X. W. Wang, H. J. Zhang, and S. Gao, J. Am. Chem. Soc. 2009, 131, 11650.
;
_refine_diff_density_max         5.562
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_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
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_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0637
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0658P)^2^+548.5780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1525
_refine_ls_wR_factor_ref         0.1561
_reflns_number_gt                6159
_reflns_number_total             6944
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt00002d.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'__diffrn_measurement_device_type' tag replaced with
'_diffrn_measurement_device_type'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      R-3
_cod_original_formula_sum        C94.4H58.4Cl31.2Cu6I6N24
_cod_database_code               7019048