Anion-driven conformation control and enhanced sulfate binding utilising aryl linked salicylaldoxime dicopper helicates.
Stevens, James R.; Plieger, Paul G.; Dalton transactions (Cambridge, England : 2003) 40 (2011) 12235–12241; doi:10.1039/c1dt10808e

data_7017227
_publ_section_title
;
 Anion-driven conformation control and enhanced sulfate binding utilising
 aryl linked salicylaldoxime dicopper helicates.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12235
_journal_page_last               12241
_journal_paper_doi               10.1039/c1dt10808e
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         '2(C68 H84 Cu2 N8 O8), 0.5(C2 H2 Cl6)'
_chemical_formula_sum            'C137 H169 Cl3 Cu4 N16 O16'
_chemical_formula_weight         2656.39
_chemical_name_systematic
;
?
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.474(7)
_cell_angle_beta                 98.589(7)
_cell_angle_gamma                113.012(8)
_cell_formula_units_Z            1
_cell_length_a                   11.4781(3)
_cell_length_b                   14.4375(3)
_cell_length_c                   25.0402(18)
_cell_measurement_reflns_used    19842
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      72.0
_cell_measurement_theta_min      6.6
_cell_volume                     3744.1(4)
_computing_cell_refinement
;
Rigaku CrystalClear-SM Expert 2.0 rc14
;
_computing_data_collection
;
Rigaku CrystalClear-SM Expert 2.0 rc14
;
_computing_data_reduction
;
Rigaku CrystalClear-SM Expert 2.0 rc14
;
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type
;
Rigaku CrystalClear-SM Expert 2.0 rc14
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0686
_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       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            48836
_diffrn_reflns_theta_full        62.38
_diffrn_reflns_theta_max         62.38
_diffrn_reflns_theta_min         6.57
_exptl_absorpt_coefficient_mu    1.620
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.389
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1398
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.17
_platon_squeeze_details
;
47 electrons per cell were squeezed.
This corresponds approximately to an iso-propyl
molecule per cell (56 e-).

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

>>> The Following Model and Quality ALERTS were generated <<<
Format: alert-number_ALERT_alert-type_alert-level text

910_ALERT_3_A # Missing FCF Reflections Below Th(Min) ........ 23
023_ALERT_3_C Resolution (too) Low [sin(theta)/Lambda < 0.6].. 62.38 Deg.
029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98
230_ALERT_2_C Hirshfeld Test Diff for N8 -- C39 .. 6.24 su
230_ALERT_2_C Hirshfeld Test Diff for C33 -- C44 .. 6.51 su
242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C42
341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 7
911_ALERT_3_C # Missing FCF Refl Between THmin & STh/L= 0.575 225

Noted
;
_refine_diff_density_max         1.155
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     812
_refine_ls_number_reflns         11657
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0761
_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^)+(0.1503P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2241
_refine_ls_wR_factor_ref         0.2462
_reflns_number_gt                8137
_reflns_number_total             11657
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10808e.txt
_cod_data_source_block           rl6
_cod_depositor_comments
;
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_cell_volume        3744.1(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7017227