Synthesis of a self-assembled copper(ii) metallo-rectangle with a guanosine-substituted terpyridine.
Ghosh, Sushobhan; Silber, Georg T.; White, Andrew J. P.; Robertson, Neil; Vilar, Ramon; Dalton transactions (Cambridge, England : 2003) 42 (2013) 13813–13816; doi:10.1039/c3dt51845k

data_7021982
_publ_section_title
;
 Synthesis of a self-assembled copper(ii) metallo-rectangle with a
 guanosine-substituted terpyridine.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13813
_journal_page_last               13816
_journal_paper_doi               10.1039/c3dt51845k
_journal_volume                  42
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C60 H64 Cu2 N16 O14, 4(N O3), 4(C H4 O), 3(H2 O)'
_chemical_formula_sum            'C64 H86 Cu2 N20 O33'
_chemical_formula_weight         1790.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.893(3)
_cell_angle_beta                 103.008(3)
_cell_angle_gamma                94.397(3)
_cell_formula_units_Z            1
_cell_length_a                   10.2878(3)
_cell_length_b                   13.7254(5)
_cell_length_c                   14.8599(5)
_cell_measurement_reflns_used    7485
_cell_measurement_temperature    173
_cell_measurement_theta_max      72.3066
_cell_measurement_theta_min      3.2357
_cell_volume                     1921.34(12)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 8.2556
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'OD Xcalibur PX Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15137
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         72.46
_diffrn_reflns_theta_min         3.24
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.574
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_correction_T_min  0.723
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) 
(compiled Aug  3 2011,13:03:54) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablets
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
 SQUEEZE suggested 103 e/cell
 The solvent used was a methanol (CH4O = 18e)/water (H2O = 10e) mixture.
 The solvent before SQUEEZE looked like a mix of methanol and water.
 4MeOH.3H2O = (4x18)+(3x10) = 102e so this was used as the solvent present.
 
 Thus UNIT is low by 4(CH4O) + 3(H2O) = C4 H22 O7,
 i.e. C60 H64 N20 O26 Cu2
;
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 1936 Friedel pairs'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1090
_refine_ls_number_reflns         9357
_refine_ls_number_restraints     243
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1024P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1395
_reflns_number_gt                8276
_reflns_number_total             9357
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51845k.txt
_cod_data_source_block           3
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P1
_cod_database_code               7021982