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_7019049
_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            'C266.5 H195 Cl29 Cu12 N96 O84'
_chemical_formula_weight         7876.86
_chemical_name_systematic
;
?
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   25.626(7)
_cell_length_b                   25.626(7)
_cell_length_c                   85.61(3)
_cell_measurement_reflns_used    45241
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.1
_cell_measurement_theta_min      2.1
_cell_volume                     48687(3)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)'
_computing_data_reduction
'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_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \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  0.0672
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       101
_diffrn_reflns_limit_l_min       -101
_diffrn_reflns_number            120649
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    1.070
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.844
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            dark-brow
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             23322
_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 4370, is included in the formula, formula weight, calculated density, and F(000). These residual electron density were assigned to 12 water molecules and 14.5 dichloromethane molecules. So SQUEEZE 12 water molecules and 14.5 dichloromethane molecules per formula unit. This value calculated based upon electrons analysis. (One water molecule would give 10 e; one dichloromethane molecule would give 42 e). So the tentative formula for this compound is presented as in the text.
See refs. (a) C. H Tan, S. H Yang, N. R. Champness, X. Lin, A. J. Blake, W. Lewis and M. Schroder, Chem. Commun., 2011, 47, 4487; (b) A. L. Spek, Acta Crystallogr.Sect.D, 2009, 65, 148.
Z before the SQUEEZE is 6 and after the SQUEEZE is 12
;
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     737
_refine_ls_number_reflns         9550
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.209
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0784
_refine_ls_shift/su_max          0.074
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+602.7534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1696
_refine_ls_wR_factor_ref         0.1737
_reflns_number_gt                8689
_reflns_number_total             9550
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt00002d.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_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_cell_volume        48687(25)
_cod_original_sg_symbol_H-M      R-3c
_cod_original_formula_sum        C266.5H195Cl29Cu12N96O84
_cod_database_code               7019049