# Electronic Supplementary Material (ESI) for Nanoscale.
# This journal is © The Royal Society of Chemistry 2014

data_ST1001
_audit_creation_date        "12-10-02"
_audit_creation_method CRYSTALS_ver_14.40
 
_publ_contact_author_name         'Stephen A. Moggach' 
_publ_contact_author_address 
; 
 Dr Stephen Moggach 
 RSE Personal Research Fellow 
 The University of Edinburgh 
 Joseph Black Building 
 West Mains Road 
 Edinburgh 
 EH9 3JJ 
; 
 
_publ_contact_author_phone        '+44(0)131 6504806' 
_publ_contact_author_email        'smoggach@staffmail.ed.ac.uk' 
 
_publ_section_exptl_refinement 
;

#===============================================================================

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


601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of .        209 Ang3 
044_ALERT_1_B Calculated and Reported Dx Differ ..............          ?
043_ALERT_1_C Check Reported Molecular Weight ................     965.18
041_ALERT_1_G Calc. and Reported SumFormula    Strings  Differ          ?
042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ          ?
8_ALERT_1_G Reported F000 Differs from Calcd (or Missing)...          ?

Structure is a porous framework with disordered solvent in the pores.
The solvent region was treated by the van der Sluis and Spek method, accounting
for 3 water molecules per formula unit. See below.
F(000), M, mu, D and the given formulae have been calculated on this assumption.


301_ALERT_3_B Note: Main Residue  Disorder ...................          5 % 

C7 Ester groups are disordered

    
341_ALERT_3_B Low Bond Precision on  C-C Bonds ...............       5.00 Ang.
220_ALERT_2_G Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       3.99 Ratio 
250_ALERT_2_G Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.53

Structure is a large porous framework collected at room temperature, 
with weak diffraction at high angle. Thermal motion is to be expected, 
especially for atoms 'pointing into the pore'
  
 
779_ALERT_4_B Suspect or Irrelevant (Bond) Angle in CIF .... #                
              H71  -C7   -H71    12.558   1.555   1.555      

Not a real bond  


045_ALERT_1_G Calculated and Reported Z Differ by ............       3.00 Ratio 

This reflects the choice of formula unit


241_ALERT_2_G Check High      Ueq as Compared to Neighbors for         O2     
242_ALERT_2_G Check Low       Ueq as Compared to Neighbors for        Cu1

O2 is adjacent to the heavy atom Cu1  


731_ALERT_1_G Bond    Calc    1.250(7), Rep    1.251(3) ......          2 su-Rat
              O1   -C1      1.555   1.555                                       
732_ALERT_1_G Angle   Calc    119.9(4), Rep  119.93(18) ......       2.22 su-Rat
              C1   -C2   -C3      1.555   1.555   1.555   

The use of restraints in the refinement mean that off diagonal terms in the
variance-covariance matrix are significant, and the diagonal approximation
used in Platon/Checkcif is badly in error.

764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) .       1.07 Ratio 

No action taken

#===============================================================================
; 

loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000 -0.008       209        14 ' '
   2  0.333  0.667 -0.053       142        33 ' '
   3  0.667  0.333  0.004       142        33 ' '
_platon_squeeze_details
;
see above for details
;
 
_publ_section_exptl_prep 
# Brief details or a reference. Include solvent if known 
; 
? 
; 
 
_cell_length_a                    18.6500(17)
_cell_length_b                    18.6500(17)
_cell_length_c                    6.8329(9)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      2058.2(4)
 
_symmetry_cell_setting            'trigonal' 
_symmetry_space_group_name_H-M    'P -3 m 1 ' 
_symmetry_space_group_name_Hall   '-P 3 2"' 
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 '-x,-y,-z'
 '-y,x-y,z'
 'y,-x+y,-z'
 '-x+y,-x,z'
 'x-y,x,-z'
 '-x+y,y,z'
 'x-y,-y,-z'
 'x,x-y,z'
 '-x,-x+y,-z'
 '-y,-x,z'
 'y,x,-z'

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source  
 C       0.0033   0.0016   2.3100  20.8439   1.0200  10.2075   1.5886   0.5687
   0.8650  51.6512   0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 H       0.0000   0.0000   0.4930  10.5109   0.3229  26.1257   0.1402   3.1424
   0.0408  57.7998   0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 O       0.0106   0.0060   3.0485  13.2771   2.2868   5.7011   1.5463   0.3239
   0.8670  32.9089   0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 Cu      0.3201   1.2651  13.3380   3.5828   7.1676   0.2470   5.6158  11.3966
   1.6735  64.8126   1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 
 
_cell_formula_units_Z                    2

# Given Formula = C33 H33 Cu3 O26.00 
# Dc =      1.67 Fooo =    918.00 Mu =     16.31 M =    172.71
# Found Formula = C30 H24 Cu3 O21 
# Dc =      1.47 FOOO =    918.00 Mu =     16.11 M =    151.86

_chemical_formula_sum             'C30 H30 Cu3 O24'
_chemical_formula_moiety          'C30 H24 Cu3 O21.3H2O'
_chemical_compound_source                ?
_chemical_formula_weight            965.185
 
 
_cell_measurement_reflns_used         9989
_cell_measurement_theta_min              3
_cell_measurement_theta_max             27
_cell_measurement_temperature          300
 
_exptl_crystal_description        'block' 
_exptl_crystal_colour             'blue' 
_exptl_crystal_size_min           0.060 
_exptl_crystal_size_mid           0.070 
_exptl_crystal_size_max           0.110 
 
_exptl_crystal_density_diffrn     1.557 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              978
_exptl_absorpt_coefficient_mu     1.62
 
# Sheldrick geometric approximatio 0.89 0.91 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'SADABS (Siemens, 1996)' 
_exptl_absorpt_correction_T_min   0.83 
_exptl_absorpt_correction_T_max   0.91 
_diffrn_measurement_device_type   'Bruker Kappa Apex2' 
_diffrn_measurement_device        'Area' 
_diffrn_radiation_monochromator   'graphite' 
_diffrn_radiation_type            'Mo K\a'
_diffrn_radiation_wavelength           0.71073
_diffrn_measurement_method        ω 
 
# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection        'Apex2 (Bruker AXS, 2006)' 
_computing_cell_refinement        'Apex2 (Bruker AXS, 2006)' 
_computing_data_reduction         'SAINT (Siemens ,1995)' 
_computing_structure_solution     'SHELXS 86 (Sheldrick, 1986)' 
_computing_structure_refinement   'CRYSTALS (Betteridge et al., 2003)' 
_computing_publication_material   'CRYSTALS (Betteridge et al., 2003)' 
_computing_molecular_graphics     'CAMERON (Watkin et al., 1996)' 
 
_diffrn_standards_interval_time   . 
_diffrn_standards_interval_count  . 
_diffrn_standards_number          0 
_diffrn_standards_decay_%         ? 
 
_diffrn_ambient_temperature        300
_diffrn_reflns_number             22534 
_reflns_number_total              1832 
_diffrn_reflns_av_R_equivalents   0.042 
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 1832 
# Theoretical number of reflections is about 3459 
 
 
_diffrn_reflns_theta_min          1.261 
_diffrn_reflns_theta_max          28.443 
_diffrn_measured_fraction_theta_max 0.968 
 
_diffrn_reflns_theta_full         26.167 
_diffrn_measured_fraction_theta_full 0.997 
 
 
_diffrn_reflns_limit_h_min        -21 
_diffrn_reflns_limit_h_max        0 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        24 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        9 
_reflns_limit_h_min               -21 
_reflns_limit_h_max               0 
_reflns_limit_k_min               0 
_reflns_limit_k_max               24 
_reflns_limit_l_min               0 
_reflns_limit_l_max               9 
 
_oxford_diffrn_Wilson_B_factor    1.60 
_oxford_diffrn_Wilson_scale       55.72 
 
_atom_sites_solution_primary      direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    difmap
 
_refine_diff_density_min          -0.61 
_refine_diff_density_max          0.54 
 
 
# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 
 
 
# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref     I>-10.0\s(I)
_refine_ls_number_reflns          1832 
_refine_ls_number_restraints      4 
_refine_ls_number_parameters      96 
_oxford_refine_ls_R_factor_ref    0.0451 
_refine_ls_wR_factor_ref          0.0847 
_refine_ls_goodness_of_fit_ref    0.9395 
_refine_ls_shift/su_max           0.0051845 
_refine_ls_shift/su_mean          0.0001453 
 
 
# The values computed with all filters except I/sigma 
_oxford_reflns_number_all         1832 
_refine_ls_R_factor_all           0.0451 
_refine_ls_wR_factor_all          0.0847 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0σ(I)
_reflns_number_gt                 1411 
_refine_ls_R_factor_gt            0.0318 
_refine_ls_wR_factor_gt           0.0808 
 
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration  '.' 
 
 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full
_refine_ls_hydrogen_treatment     constr         #undef, noref, refall,
                                                 # refxyz, refU, constr or mixed
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.04P)² + 2.43P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
# Insert your own references if required - in alphabetical order 
_publ_section_references 
; 
Betteridge, P.W., Carruthers, J.R., Cooper, R.I., 
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 
 
Bruker Analytical X-ray Systems, Inc., 2006. Apex2, 
Version 2 User Manual, M86-E01078, Madison, WI. 
 
Sheldrick, G. M. (2008). Acta Cryst A64, 112-122. 
 
Siemens Industrial Automation, Inc (1995). 
SAINT: Area-Detector Integration Software.; Madison, WI. 
 
Siemens Industrial Automation, Inc (1996). 
SADABS: Area-Detector Absorption Correction;: Madison, WI. 
 
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical 
Crystallography Laboratory, Oxford, UK. 
; 

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cu1 Cu 0.523326(12) 0.476674(12) 0.34460(6) 0.0219 1.0000 Uani S T . . . . 
O1 O 0.2847(2) 0.2017(2) 1.2482(4) 0.0968 1.0000 Uani . . . . . . 
O2 O 0.48066(14) 0.37132(12) 0.4816(3) 0.0434 1.0000 Uani . . . . . . 
O3 O 0.44207(14) 0.41094(12) 0.7487(3) 0.0414 1.0000 Uani . . . . . . 
O4 O 0.56158(9) 0.43842(9) 0.0889(4) 0.0488 1.0000 Uani DS T . . . . 
H42 H 0.5244 0.4175 0.0130 0.0600 1.0000 Uiso DR . . . . . 
C1 C 0.3046(4) 0.15230(18) 1.1773(7) 0.0573 1.0000 Uani S T . . . . 
C2 C 0.3551(3) 0.17755(14) 0.9970(6) 0.0415 1.0000 Uani S T . . . . 
C3 C 0.37859(19) 0.25389(18) 0.9120(4) 0.0380 1.0000 Uani . . . . . . 
C4 C 0.42298(17) 0.27630(16) 0.7391(4) 0.0308 1.0000 Uani . . . . . . 
C5 C 0.4438(2) 0.22188(12) 0.6513(5) 0.0307 1.0000 Uani S T . . . . 
C6 C 0.45021(16) 0.35905(16) 0.6490(4) 0.0283 1.0000 Uani . . . . . . 
C7 C 0.2352(8) 0.1866(7) 1.4178(14) 0.1130 0.5000 Uani . . . . . . 
H31 H 0.3674 0.2918 0.9792 0.0600 1.0000 Uiso R . . . . . 
H51 H 0.4738 0.2369 0.5318 0.0600 1.0000 Uiso RS . . . . . 
H71 H 0.2285 0.2347 1.4413 0.1264 0.5000 Uiso R . . . . . 
H72 H 0.2638 0.1790 1.5292 0.1264 0.5000 Uiso R . . . . . 
H73 H 0.1807 0.1371 1.4018 0.1264 0.5000 Uiso R . . . . . 
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0249(2) 0.0249(2) 0.0222(2) 0.00026(8) -0.00026(8) 0.01701(19) 
O1 0.142(3) 0.088(2) 0.087(2) 0.0243(18) 0.073(2) 0.078(2) 
O2 0.0708(15) 0.0328(11) 0.0351(10) 0.0088(9) 0.0168(10) 0.0323(11) 
O3 0.0667(14) 0.0283(10) 0.0367(10) 0.0076(8) 0.0147(10) 0.0295(10) 
O4 0.0659(16) 0.0659(16) 0.0295(14) -0.0033(7) 0.0033(7) 0.0441(19) 
C1 0.079(4) 0.0488(19) 0.055(3) 0.0167(13) 0.033(3) 0.0393(19) 
C2 0.053(3) 0.0331(14) 0.045(2) 0.0108(10) 0.022(2) 0.0264(13) 
C3 0.0483(18) 0.0326(15) 0.0419(15) 0.0056(12) 0.0138(14) 0.0268(14) 
C4 0.0364(15) 0.0256(13) 0.0342(13) 0.0021(11) 0.0030(12) 0.0185(12) 
C5 0.038(2) 0.0267(13) 0.0314(19) 0.0022(8) 0.0045(16) 0.0189(11) 
C6 0.0298(13) 0.0261(13) 0.0338(13) 0.0021(11) -0.0007(11) 0.0176(11) 
C7 0.153(11) 0.115(9) 0.080(6) -0.002(6) 0.044(7) 0.073(9) 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 0.13916(9) 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
Cu1 . O3 2_666 1.9655(18)    yes
Cu1 . O3 12_556 1.9655(18)    yes
Cu1 . O2 11_665 1.9510(19)    yes
Cu1 . Cu1 2_666 2.6040(8)    yes
Cu1 . O2 . 1.9510(19)    yes
Cu1 . O4 . 2.140(3)    yes
O1 . C1 . 1.251(3)    yes
O1 . C7 . 1.418(9)    yes
O2 . C6 . 1.246(3)    yes
O3 . C6 . 1.253(3)    yes
O4 . H42 11_665 0.794    no
O4 . H42 . 0.794    no
C1 . C2 . 1.477(6)    yes
C2 . C3 9_555 1.390(3)    yes
C2 . C3 . 1.390(3)    yes
C3 . C4 . 1.382(4)    yes
C3 . H31 . 0.950    no
C4 . C5 . 1.391(3)    yes
C4 . C6 . 1.495(3)    yes
C5 . H51 . 0.950    no
C7 . H71 12_558 1.243    no
C7 . H71 . 0.980    no
C7 . H72 . 0.980    no
C7 . H73 . 0.980    no
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
O3 2_666 Cu1 . O3 12_556 88.43(13)    yes
O3 2_666 Cu1 . O2 11_665 89.65(10)    yes
O3 12_556 Cu1 . O2 11_665 168.71(8)    yes
O3 2_666 Cu1 . Cu1 2_666 83.95(6)    yes
O3 12_556 Cu1 . Cu1 2_666 83.95(6)    yes
O2 11_665 Cu1 . Cu1 2_666 84.79(6)    yes
O3 2_666 Cu1 . O2 . 168.71(8)    yes
O3 12_556 Cu1 . O2 . 89.65(10)    yes
O2 11_665 Cu1 . O2 . 90.06(14)    yes
Cu1 2_666 Cu1 . O2 . 84.79(6)    yes
O3 2_666 Cu1 . O4 . 95.98(8)    yes
O3 12_556 Cu1 . O4 . 95.99(8)    yes
O2 11_665 Cu1 . O4 . 95.28(8)    yes
Cu1 2_666 Cu1 . O4 . 179.91(8)    yes
O2 . Cu1 . O4 . 95.28(8)    yes
C1 . O1 . C7 . 124.9(5)    yes
Cu1 . O2 . C6 . 122.96(17)    yes
Cu1 2_666 O3 . C6 . 123.03(17)    yes
Cu1 . O4 . H42 11_665 110.0    no
Cu1 . O4 . H42 . 110.0    no
H42 11_665 O4 . H42 . 86.0    no
O1 9_555 C1 . O1 . 124.6(5)    yes
O1 9_555 C1 . C2 . 117.7(2)    yes
O1 . C1 . C2 . 117.7(2)    yes
C1 . C2 . C3 9_555 119.93(18)    yes
C1 . C2 . C3 . 119.93(18)    yes
C3 9_555 C2 . C3 . 120.1(4)    yes
C2 . C3 . C4 . 120.1(3)    yes
C2 . C3 . H31 . 119.1    no
C4 . C3 . H31 . 120.6    no
C3 . C4 . C5 . 119.4(3)    yes
C3 . C4 . C6 . 120.5(2)    yes
C5 . C4 . C6 . 120.1(2)    yes
C4 . C5 . C4 9_555 120.7(3)    yes
C4 . C5 . H51 . 119.6    no
C4 9_555 C5 . H51 . 119.6    no
C4 . C6 . O3 . 117.6(2)    yes
C4 . C6 . O2 . 117.1(2)    yes
O3 . C6 . O2 . 125.3(2)    yes
O1 . C7 . H71 12_558 135.7    no
O1 . C7 . H71 . 108.7    no
H71 12_558 C7 . H71 . 41.6    no
O1 . C7 . H72 . 108.5    no
H71 12_558 C7 . H72 . 70.4    no
H71 . C7 . H72 . 109.5    no
O1 . C7 . H73 . 111.2    no
H71 12_558 C7 . H73 . 110.4    no
H71 . C7 . H73 . 109.5    no
H72 . C7 . H73 . 109.5    no
C7 . H71 . C7 12_558 120.2    no


_iucr_refine_instruction_details_constraints
;
#
# Punched on 02/10/12 at 10:49:28
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT H(42, X'S) 
RIDE O   (   4,X'S) H   (  42,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) H   (  72,X'S) H   (  73,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints
;
#
# Punched on 02/10/12 at 10:49:28
#
#LIST     16                                                                    
DIST 0.84, 0.01 = O(4) TO H(42) 
ANGLE 108, 1 = H(42) TO O(4) TO H(42,6,1,1,1) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

#===END

data_ST1002
_audit_creation_date        "12-10-02"
_audit_creation_method CRYSTALS_ver_14.40
 
_publ_contact_author_name         'Stephen A. Moggach' 
_publ_contact_author_address 
; 
 Dr Stephen Moggach 
 RSE Personal Research Fellow 
 The University of Edinburgh 
 Joseph Black Building 
 West Mains Road 
 Edinburgh 
 EH9 3JJ 
; 
 
_publ_contact_author_phone        '+44(0)131 6504806' 
_publ_contact_author_email        'smoggach@staffmail.ed.ac.uk' 

;
#===============================================================================

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

023_ALERT_3_B Resolution (too) Low [sin(theta)/Lambda < 0.6]..      20.81 Deg.  
027_ALERT_3_B _diffrn_reflns_theta_full (too) Low ............      15.81 Deg.  
029_ALERT_3_B _diffrn_measured_fraction_theta_full Low .......       0.92       
088_ALERT_3_B Poor Data / Parameter Ratio ....................       4.58  
341_ALERT_3_B Low Bond Precision on  C-C Bonds ...............      16.00 Ang.  
731_ALERT_1_B Bond    Calc     0.83(8), Rep    0.839(9) ......          9 su-Rat
              O4   -H4      1.555   1.555  
022_ALERT_3_C Ratio Unique / Expected Reflections (too) Low ..       0.88  

The high pressure cell causes shading of a significant proportion of the
sphere of reflections. This means that the completeness is reduced and as
such the quality of the model is lower.All of the above are cause by shading 
by the pressure cell.


601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of .        238 Ang3 
043_ALERT_1_C Check Reported Molecular Weight ................    1001.28       
044_ALERT_1_C Calculated and Reported Dx Differ ..............          ?
041_ALERT_1_G Calc. and Reported SumFormula    Strings  Differ          ?
042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ          ?
068_ALERT_1_G Reported F000 Differs from Calcd (or Missing)...          ?
094_ALERT_2_G Ratio of Maximum / Minimum Residual Density ....       3.03  

Structure is a porous framework with disordered solvent in the pores.
The solvent region was treated by the van der Sluis and Spek method. 
See below. This corresponds to 1.5 molecules of methanol per formula unit. 
F(000), M, mu, D and the given formulae have been calculated on this 
assumption.
     

301_ALERT_3_B Note: Main Residue  Disorder ...................          5 %
220_ALERT_2_G Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       3.48 Ratio 

This is caused by C7 which is disordered and subject to thermal motion.
Half occupied carbon refined anistropically


199_ALERT_1_B Check the Reported _cell_measurement_temperature        293 K     
200_ALERT_1_B Check the Reported   _diffrn_ambient_temperature        293 K 

This is correct 

045_ALERT_1_G Calculated and Reported Z Differ by ............       3.00 Ratio 

this reflects the choice of formula unit  

242_ALERT_2_G Check Low       Ueq as Compared to Neighbors for        Cu1  

Cu1 is a heavy atom 


732_ALERT_1_C Angle   Calc   117.7(13), Rep    117.7(3) ......       4.33 su-Rat
              O1   -C1   -C2      1.555   1.555   1.555
731_ALERT_1_G Bond    Calc   1.251(18), Rep    1.252(6) ......          3 su-Rat
              O1   -C1      1.555   1.555                                       
731_ALERT_1_G Bond    Calc   1.494(18), Rep    1.494(7) ......          3 su-Rat
              C1   -C2      1.555   1.555                                       
731_ALERT_1_G Bond    Calc   1.388(19), Rep    1.389(5) ......          4 su-Rat
              C2   -C3      1.555   7.655                                       
731_ALERT_1_G Bond    Calc   1.389(16), Rep    1.389(5) ......          3 su-Rat
              C2   -C3      1.555   1.555                                       
731_ALERT_1_G Bond    Calc   1.392(15), Rep    1.390(6) ......          3 su-Rat
              C4   -C5      1.555   1.555                                       
731_ALERT_1_G Bond    Calc   1.490(14), Rep    1.491(6) ......          2 su-Rat
              C4   -C6      1.555   1.555                                       
732_ALERT_1_G Angle   Calc    120.1(9), Rep    120.1(4) ......       2.25 su-Rat
              C2   -C3   -C4      1.555   1.555   1.555                         
732_ALERT_1_G Angle   Calc    119.9(9), Rep    120.0(4) ......       2.25 su-Rat
              C3   -C4   -C5      1.555   1.555   1.555                         
732_ALERT_1_G Angle   Calc    120.7(9), Rep    120.6(4) ......       2.25 su-Rat
              C3   -C4   -C6      1.555   1.555   1.555                         
752_ALERT_4_G Angle   Calc      120.00, Rep    120.0(3) ......  Senseless su    
              C1   -C2   -C3      1.555   1.555   1.555
     
The use of restraints in the refinement mean that off diagonal terms in the
variance-covariance matrix are significant, and the diagonal approximation
used in Platon/Checkcif is badly in error.
                         
764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) .       1.06 Ratio

No action taken
#===============================================================================
                        
;
 
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000 -0.013       283        51 ' '
   2  0.333  0.667  0.464        46        11 ' '
   3  0.667  0.333  0.536        46        11 ' '
_platon_squeeze_details
;
see above for details
;

_publ_section_exptl_refinement 
; 
; 
 
_publ_section_exptl_prep 
# Brief details or a reference. Include solvent if known 
; 
? 
; 
 
_cell_length_a                    18.695(3)
_cell_length_b                    18.695(3)
_cell_length_c                    6.9489(9)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      2103.2(5)
 
_symmetry_cell_setting            'trigonal' 
_symmetry_space_group_name_H-M    'P -3 m 1 ' 
_symmetry_space_group_name_Hall   '-P 3 2"'
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 '-x,-y,-z'
 '-y,x-y,z'
 'y,-x+y,-z'
 '-x+y,-x,z'
 'x-y,x,-z'
 '-x+y,y,z'
 'x-y,-y,-z'
 'x,x-y,z'
 '-x,-x+y,-z'
 '-y,-x,z'
 'y,x,-z'

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source  
 C       0.0033   0.0016   2.3100  20.8439   1.0200  10.2075   1.5886   0.5687
   0.8650  51.6512   0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 H       0.0000   0.0000   0.4930  10.5109   0.3229  26.1257   0.1402   3.1424
   0.0408  57.7998   0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 O       0.0106   0.0060   3.0485  13.2771   2.2868   5.7011   1.5463   0.3239
   0.8670  32.9089   0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 Cu      0.3201   1.2651  13.3380   3.5828   7.1676   0.2470   5.6158  11.3966
   1.6735  64.8126   1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 
 
_cell_formula_units_Z                    2

# Given Formula = C9 H7 Cu1 O8.00 
# Dc =      1.94 Fooo =    966.00 Mu =     21.10 M =    204.46
# Found Formula = C8.25 H7.50 Cu0.75 O5.25 
# Dc =      1.51 FOOO =    966.00 Mu =     15.81 M =    158.87

_chemical_formula_sum             'C34.5 H36 Cu3 O22.5 '
_chemical_formula_moiety          'C33 H30 Cu3 O21.1.5CH3OH'
_chemical_compound_source                ?
_chemical_formula_weight            1001.28
 
 
_cell_measurement_reflns_used         1422 
_cell_measurement_theta_min              3
_cell_measurement_theta_max             27
_cell_measurement_temperature          293
 
_exptl_crystal_description        'block' 
_exptl_crystal_colour             'blue' 
_exptl_crystal_size_min           0.060 
_exptl_crystal_size_mid           0.070 
_exptl_crystal_size_max           0.110 
 
_exptl_crystal_density_diffrn     1.581 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              1020
_exptl_absorpt_coefficient_mu     1.59 
 
# Sheldrick geometric approximatio 1.00 1.00 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'SADABS (Siemens, 1996)' 
_exptl_absorpt_correction_T_min   0.89
_exptl_absorpt_correction_T_max   0.91 
_diffrn_measurement_device_type   'Bruker Kappa Apex2' 
_diffrn_measurement_device        'Area' 
_diffrn_radiation_monochromator   'graphite' 
_diffrn_radiation_type            'Mo K\a'
_diffrn_radiation_wavelength           0.71073
_diffrn_measurement_method        ω 
 
# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection        'Apex2 (Bruker AXS, 2006)' 
_computing_cell_refinement        'Apex2 (Bruker AXS, 2006)' 
_computing_data_reduction         'Apex2 (Bruker AXS, 2006)' 
_computing_structure_solution     'USER DEFINED STRUCTURE SOLUTION' 
_computing_structure_refinement   'CRYSTALS (Betteridge et al., 2003)' 
_computing_publication_material   'CRYSTALS (Betteridge et al., 2003)' 
_computing_molecular_graphics     'CAMERON (Watkin et al., 1996)' 
 
_diffrn_standards_interval_time   . 
_diffrn_standards_interval_count  . 
_diffrn_standards_number          0 
_diffrn_standards_decay_%         ? 
 
_diffrn_ambient_temperature        293
_diffrn_reflns_number             4723 
_reflns_number_total              725 
_diffrn_reflns_av_R_equivalents   0.119 
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 725 
# Theoretical number of reflections is about 1448 
 
 
_diffrn_reflns_theta_min          3.190 
_diffrn_reflns_theta_max          20.805 
_diffrn_measured_fraction_theta_max 0.880 
 
_diffrn_reflns_theta_full         15.812 
_diffrn_measured_fraction_theta_full 0.920 
 
 
_diffrn_reflns_limit_h_min        -18 
_diffrn_reflns_limit_h_max        15 
_diffrn_reflns_limit_k_min        -16 
_diffrn_reflns_limit_k_max        17 
_diffrn_reflns_limit_l_min        -6 
_diffrn_reflns_limit_l_max        6 
_reflns_limit_h_min               -16 
_reflns_limit_h_max               0 
_reflns_limit_k_min               0 
_reflns_limit_k_max               18 
_reflns_limit_l_min               0 
_reflns_limit_l_max               6 
 
_oxford_diffrn_Wilson_B_factor    1.71 
_oxford_diffrn_Wilson_scale       111.94 
 
_atom_sites_solution_primary      Other  #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    difmap
 
_refine_diff_density_min          -0.63 
_refine_diff_density_max          1.91 
 
 
# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 
 
 
# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref     I>2.0\s(I)
_refine_ls_number_reflns          467 
_refine_ls_number_restraints      119 
_refine_ls_number_parameters      102 
_oxford_refine_ls_R_factor_ref    0.0730 
_refine_ls_wR_factor_ref          0.0797 
_refine_ls_goodness_of_fit_ref    1.0888 
_refine_ls_shift/su_max           0.0001609 
_refine_ls_shift/su_mean          0.0000194 
 
 
# The values computed with all filters except I/sigma 
_oxford_reflns_number_all         685 
_refine_ls_R_factor_all           0.1160 
_refine_ls_wR_factor_all          0.1452 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0σ(I)
_reflns_number_gt                 467 
_refine_ls_R_factor_gt            0.0730 
_refine_ls_wR_factor_gt           0.0797 
 
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration  '.' 
 
 
_refine_ls_structure_factor_coef  F 
_refine_ls_matrix_type            full
_refine_ls_hydrogen_treatment     mixed          #undef, noref, refall,
                                                 # refxyz, refU, constr or mixed
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.882 0.459 0.520 
;
# Insert your own references if required - in alphabetical order 
_publ_section_references 
; 
User-defined structure solution reference 
 
Betteridge, P.W., Carruthers, J.R., Cooper, R.I., 
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 
 
Bruker Analytical X-ray Systems, Inc., 2006. Apex2, 
Version 2 User Manual, M86-E01078, Madison, WI. 
 
Prince, E. 
Mathematical Techniques in Crystallography 
and Materials Science 
Springer-Verlag, New York, 1982. 
 
Siemens Industrial Automation, Inc (1996). 
SADABS: Area-Detector Absorption Correction;: Madison, WI. 
 
Watkin D.J. (1994). 
Acta Cryst, A50, 411-437. 
 
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical 
Crystallography Laboratory, Oxford, UK. 
; 

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cu1 Cu 0.52264(6) 0.47736(6) 0.3452(2) 0.0256 1.0000 Uani S T . . . . 
O1 O 0.9112(5) 0.7039(6) 1.2514(12) 0.0845 1.0000 Uani D U . . . . 
O2 O 0.6287(4) 0.5175(5) 0.4782(9) 0.0422 1.0000 Uani D U . . . . 
O3 O 0.5899(4) 0.5562(5) 0.7417(9) 0.0470 1.0000 Uani D U . . . . 
O4 O 0.5565(3) 0.4435(3) 0.0870(13) 0.0436 1.0000 Uani DS TU . . . . 
C1 C 0.8438(6) 0.6877(11) 1.1763(17) 0.0572 1.0000 Uani DS TU . . . . 
C2 C 0.8193(5) 0.6385(9) 0.9944(15) 0.0401 1.0000 Uani DS TU . . . . 
C3 C 0.7442(4) 0.6170(7) 0.9078(12) 0.0394 1.0000 Uani D U . . . . 
C4 C 0.7233(4) 0.5754(7) 0.7324(11) 0.0313 1.0000 Uani D U . . . . 
C5 C 0.7775(4) 0.5551(9) 0.6441(14) 0.0277 1.0000 Uani DS TU . . . . 
C6 C 0.6411(5) 0.5479(7) 0.6431(10) 0.0357 1.0000 Uani D U . . . . 
C7 C 0.9481(14) 0.7556(19) 1.416(3) 0.0971 0.5000 Uani D U . . . . 
C8 C 0.5990(4) 0.4010(4) 0.068(3) 0.0648 1.0000 Uani DS TU . . . . 
H4 H 0.535(3) 0.465(3) 0.021(19) 0.0500 1.0000 Uiso DS . . . . . 
H31 H 0.7071 0.6309 0.9680 0.0469 1.0000 Uiso . . . . . . 
H51 H 0.7636 0.5273 0.5237 0.0330 1.0000 Uiso . . . . . . 
H71 H 1.0004 0.7578 1.4461 0.1125 0.5000 Uiso . . . . . . 
H72 H 0.9579 0.8109 1.3898 0.1125 0.5000 Uiso . . . . . . 
H73 H 0.9105 0.7320 1.5268 0.1125 0.5000 Uiso . . . . . . 
H81 H 0.6061 0.3939 -0.0700 0.0759 1.0000 Uiso . . . . . . 
H82 H 0.5676 0.3468 0.1285 0.0759 1.0000 Uiso . . . . . . 
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0288(13) 0.0288(13) 0.0265(11) 0.0009(4) -0.0009(4) 0.0198(13) 
O1 0.068(7) 0.105(9) 0.082(6) -0.051(5) -0.039(5) 0.044(7) 
O2 0.032(5) 0.057(6) 0.046(4) -0.011(3) -0.004(3) 0.028(5) 
O3 0.035(5) 0.078(7) 0.047(4) -0.010(4) -0.007(3) 0.042(5) 
O4 0.064(7) 0.064(7) 0.035(6) 0.003(2) -0.003(2) 0.056(8) 
C1 0.054(6) 0.068(13) 0.054(8) -0.025(7) -0.013(3) 0.034(7) 
C2 0.034(6) 0.042(11) 0.047(7) -0.011(5) -0.006(3) 0.021(5) 
C3 0.026(6) 0.042(8) 0.053(5) -0.014(4) 0.000(4) 0.019(6) 
C4 0.026(5) 0.032(7) 0.043(5) -0.002(4) -0.001(3) 0.020(5) 
C5 0.023(4) 0.034(10) 0.029(6) 0.000(6) 0.000(3) 0.017(5) 
C6 0.028(6) 0.046(9) 0.041(4) -0.003(4) -0.002(4) 0.025(7) 
C7 0.08(2) 0.10(3) 0.068(16) -0.039(14) -0.029(13) 0.02(2) 
C8 0.077(14) 0.077(14) 0.081(12) -0.001(5) 0.001(5) 0.068(14) 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 0.1329(11) 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
Cu1 . O3 2_666 1.966(7)    yes
Cu1 . O3 12_556 1.966(7)    yes
Cu1 . O2 11_665 1.965(6)    yes
Cu1 . Cu1 2_666 2.603(3)    yes
Cu1 . O2 . 1.965(6)    yes
Cu1 . O4 . 2.102(9)    yes
O1 . C1 . 1.252(6)    yes
O1 . C7 . 1.433(8)    yes
O2 . C6 . 1.248(6)    yes
O3 . C6 . 1.248(7)    yes
O4 . C8 . 1.384(8)    yes
O4 . H4 . 0.839(9)    no
C1 . C2 . 1.494(7)    yes
C2 . C3 7_655 1.389(5)    yes
C2 . C3 . 1.389(5)    yes
C3 . C4 . 1.393(7)    yes
C3 . H31 . 0.950    no
C4 . C5 . 1.390(6)    yes
C4 . C6 . 1.491(6)    yes
C5 . H51 . 0.951    no
C7 . H72 . 0.975    no
C7 . H73 . 0.985    no
C8 . H82 11_665 0.977    no
C8 . H81 . 0.983    no
C8 . H82 . 0.977    no
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
O3 2_666 Cu1 . O3 12_556 88.0(5)    yes
O3 2_666 Cu1 . O2 11_665 90.9(3)    yes
O3 12_556 Cu1 . O2 11_665 168.8(2)    yes
O3 2_666 Cu1 . Cu1 2_666 83.6(2)    yes
O3 12_556 Cu1 . Cu1 2_666 83.6(2)    yes
O2 11_665 Cu1 . Cu1 2_666 85.27(19)    yes
O3 2_666 Cu1 . O2 . 168.8(2)    yes
O3 12_556 Cu1 . O2 . 90.9(3)    yes
O2 11_665 Cu1 . O2 . 88.1(5)    yes
Cu1 2_666 Cu1 . O2 . 85.27(19)    yes
O3 2_666 Cu1 . O4 . 94.4(3)    yes
O3 12_556 Cu1 . O4 . 94.4(3)    yes
O2 11_665 Cu1 . O4 . 96.8(3)    yes
Cu1 2_666 Cu1 . O4 . 177.1(3)    yes
O2 . Cu1 . O4 . 96.8(3)    yes
C1 . O1 . C7 . 125.7(8)    yes
Cu1 . O2 . C6 . 121.8(4)    yes
Cu1 2_666 O3 . C6 . 123.8(4)    yes
Cu1 . O4 . C8 . 127.0(9)    yes
Cu1 . O4 . H4 . 91(11)    no
C8 . O4 . H4 . 142(11)    no
O1 . C1 . O1 7_655 124.4(6)    yes
O1 . C1 . C2 . 117.7(3)    yes
O1 7_655 C1 . C2 . 117.7(3)    yes
C1 . C2 . C3 7_655 120.0(3)    yes
C1 . C2 . C3 . 120.0(3)    yes
C3 7_655 C2 . C3 . 119.9(5)    yes
C2 . C3 . C4 . 120.1(4)    yes
C2 . C3 . H31 . 120.0    no
C4 . C3 . H31 . 120.0    no
C3 . C4 . C5 . 120.0(4)    yes
C3 . C4 . C6 . 120.6(4)    yes
C5 . C4 . C6 . 119.3(4)    yes
C4 7_655 C5 . C4 . 119.9(6)    yes
C4 7_655 C5 . H51 . 120.0    no
C4 . C5 . H51 . 120.0    no
C4 . C6 . O2 . 117.6(5)    yes
C4 . C6 . O3 . 116.8(5)    yes
O2 . C6 . O3 . 125.6(5)    yes
O1 . C7 . H72 . 109.7    no
O1 . C7 . H73 . 109.1    no
H72 . C7 . H73 . 109.5    no
H82 11_665 C8 . O4 . 109.5    no
H82 11_665 C8 . H81 . 109.4    no
O4 . C8 . H81 . 109.1    no
H82 11_665 C8 . H82 . 109.9    no
O4 . C8 . H82 . 109.5    no
H81 . C8 . H82 . 109.4    no


_iucr_refine_instruction_details_constraints
;
#
# Punched on 02/10/12 at 10:41:37
#
#LIST     12                                                                    
BLOCK SCALE X'S 
CONT CU(1, U'S) UNTIL C(8) 
CONT H(4, X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints
;
#
# Punched on 02/10/12 at 10:41:37
#
#LIST     16                                                                    
DIST 0.84, 0.01 = O(4) TO H(4) 
DIST   1.39, 0.01 = O(4) TO C(8) 
DIST   1.39, 0.01 = O(5) TO C(9) 
DIST   1.258,.01= O(1) TO C(1) 
DIST   1.430,.01= O(1) TO C(7) 
DIST   1.265,.01= O(2) TO C(6) 
DIST   1.261,.01= O(3) TO C(6) 
DIST   1.499,.01= C(1) TO C(2) 
DIST   1.395,.01= C(2) TO C(3) 
DIST   1.395,.01= C(2) TO C(3,4,1,1) 
DIST   1.399,.01= C(3) TO C(4) 
DIST   1.399,.01= C(4) TO C(5) 
DIST   1.503,.01= C(4) TO C(6) 
ANGL 125,1= C(7) TO O(1) TO C(1) 
ANGL 124,1= O(1,4,1,1) TO C(1) TO O(1) 
ANGL 118,1= C(2) TO C(1) TO O(1) 
ANGL 118,1= C(2) TO C(1) TO O(1,4,1,1) 
ANGL 120,1= C(3) TO C(2) TO C(1) 
ANGL 120,1= C(3,4,1,1) TO C(2) TO C(1) 
ANGL 120,1= C(3,4,1,1) TO C(2) TO C(3) 
ANGL 120,1= C(4) TO C(3) TO C(2) 
ANGL 120,1= C(5) TO C(4) TO C(3) 
ANGL 121,1= C(6) TO C(4) TO C(3) 
ANGL 119,1= C(6) TO C(4) TO C(5) 
ANGL 120,1= C(4,4,1,1) TO C(5) TO C(4) 
ANGL 126,1= O(3) TO C(6) TO O(2) 
ANGL 117,1= C(4) TO C(6) TO O(2) 
ANGL 117,1= C(4) TO C(6) TO O(3) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = O(1) TO C(1) 
VIBR .0, 0.00200 = O(1) TO C(7) 
VIBR .0, 0.00500 = C(7) TO C(1) 
VIBR .0, 0.00200 = O(2) TO C(6) 
VIBR .0, 0.00200 = O(3) TO C(6) 
VIBR .0, 0.00200 = O(4) TO C(8) 
VIBR .0, 0.00200 = C(1) TO C(2) 
VIBR .0, 0.00500 = O(1) TO O(1,4,1,1) 
VIBR .0, 0.00500 = C(2) TO O(1,4,1,1) 
VIBR .0, 0.00500 = C(2) TO O(1) 
VIBR .0, 0.00200 = C(2) TO C(3,4,1,1) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00500 = C(3,4,1,1) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(3,4,1,1) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00200 = C(4) TO C(5) 
VIBR .0, 0.00200 = C(4) TO C(6) 
VIBR .0, 0.00500 = C(5) TO C(3) 
VIBR .0, 0.00500 = C(6) TO C(3) 
VIBR .0, 0.00500 = C(6) TO C(5) 
VIBR .0, 0.00500 = C(4) TO C(4,4,1,1) 
VIBR .0, 0.00500 = O(3) TO C(4) 
VIBR .0, 0.00500 = O(2) TO C(4) 
VIBR .0, 0.00500 = O(2) TO O(3) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = O(1) TO C(1) 
U(IJ) .0, 0.08000 = O(1) TO C(7) 
U(IJ) .0, 0.08000 = O(2) TO C(6) 
U(IJ) .0, 0.08000 = O(3) TO C(6) 
U(IJ) .0, 0.08000 = O(4) TO C(8) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.04000 = C(2) TO C(3,4,1,1) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(4) TO C(5) 
U(IJ) .0, 0.04000 = C(4) TO C(6) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
VIBRATION 0.0, 0.020000 = O(5) TO C(9) 
U(IJ)'S  0.0, 0.010000 = O(5) TO C(9) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
  -6  13   0  x   .
   0   6   1  x   .
  -7  16   2  x   .
  -8  16   3  x   .
  -7  16   3  x   .
  -6  15   0  x   .
  -7  13   1  x   .
  -4   9   0  x   .
   0   2   4  x   .

#===END

data_ST1003 
_audit_creation_date        "12-10-02"
_audit_creation_method CRYSTALS_ver_14.40


_publ_contact_author_name         'Stephen A. Moggach' 
_publ_contact_author_address 
; 
 Dr Stephen Moggach 
 RSE Personal Research Fellow 
 The University of Edinburgh 
 Joseph Black Building 
 West Mains Road 
 Edinburgh 
 EH9 3JJ 
; 
 
_publ_contact_author_phone        '+44(0)131 6504806' 
_publ_contact_author_email        'smoggach@staffmail.ed.ac.uk' 
 
;
#===============================================================================

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

601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of .        217 Ang3 
041_ALERT_1_G Calc. and Reported SumFormula    Strings  Differ          ?
042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ          ?
043_ALERT_1_G Check Reported Molecular Weight ................     969.24       
044_ALERT_1_G Calculated and Reported Dx Differ ..............          ?
068_ALERT_1_G Reported F000 Differs from Calcd (or Missing)...          ?

Structure is a porous framework with disordered solvent in the pores.
The solvent region was treated by the van der Sluis and Spek method, accounting
for 0.5 methanol molecules per formula unit. See below.
F(000), M, mu, D and the given formulae have been calculated on this assumption.


301_ALERT_3_B Note: Main Residue  Disorder ...................          5 %  

C7 is disordered   


341_ALERT_3_B Low Bond Precision on  C-C Bonds ...............       4.00 Ang. 
220_ALERT_2_G Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       3.94 Ratio
250_ALERT_2_G Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.15 
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600         11   

Structure is a large porous framework collected at room temperature, 
with weak diffraction at high angle. Thermal motion is to be expected, 
especially for atoms 'pointing into the pore'  
 
770_ALERT_2_B Suspect C-H Bond in CIF:   C7     --  H71     ..       1.31 Ang.  
779_ALERT_4_B Suspect or Irrelevant (Bond) Angle in CIF .... #                
              H71  -C7   -H71    10.768   1.555   1.555  

Not a real bond
           

045_ALERT_1_G Calculated and Reported Z Differ by ............       3.00 Ratio 

This reflects the choice of formula unit


241_ALERT_2_G Check High      Ueq as Compared to Neighbors for         O2     
242_ALERT_2_G Check Low       Ueq as Compared to Neighbors for        Cu1 

O2 is adjacent to the heavy atom Cu1  
    
      
764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) .       1.13 Ratio

NO action taken   
#===============================================================================
;
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000 -0.010       215        14 ' '
   2  0.333  0.667  0.462        48         2 ' '
   3  0.667  0.333  0.539        48         2 ' '
_platon_squeeze_details
;
see above for details
;
 
_publ_section_exptl_refinement 
; 
; 
 
_publ_section_exptl_prep 
# Brief details or a reference. Include solvent if known 
; 
? 
; 
 
_cell_length_a                    18.7034(3)
_cell_length_b                    18.7034(3)
_cell_length_c                    6.87800(10)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      2083.69(6)
 
_symmetry_cell_setting            'trigonal' 
_symmetry_space_group_name_H-M    'P -3 m 1 ' 
_symmetry_space_group_name_Hall   '-P 3 2"'
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 '-x,-y,-z'
 '-y,x-y,z'
 'y,-x+y,-z'
 '-x+y,-x,z'
 'x-y,x,-z'
 '-x+y,y,z'
 'x-y,-y,-z'
 'x,x-y,z'
 '-x,-x+y,-z'
 '-y,-x,z'
 'y,x,-z'

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source  
 C       0.0033   0.0016   2.3100  20.8439   1.0200  10.2075   1.5886   0.5687
   0.8650  51.6512   0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 O       0.0106   0.0060   3.0485  13.2771   2.2868   5.7011   1.5463   0.3239
   0.8670  32.9089   0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 Cu      0.3201   1.2651  13.3380   3.5828   7.1676   0.2470   5.6158  11.3966
   1.6735  64.8126   1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 H       0.0000   0.0000   0.4930  10.5109   0.3229  26.1257   0.1402   3.1424
   0.0408  57.7998   0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 
 
_cell_formula_units_Z                    2

# Given Formula = C59 H10 Cu3 O3 
# Dc =      1.53 Fooo =    966.00 Mu =     15.67 M =    159.56
# Found Formula = C33 H30 Cu3 O21 
# Dc =      1.52 FOOO =    966.00 Mu =     15.95 M =    158.87

_chemical_formula_sum             'C33.5 H32 Cu3 O21.5'
_chemical_formula_moiety          'C33 H30 Cu3 O21.0.5CH3OH'
_chemical_compound_source                ?
_chemical_formula_weight            969.24
 
 
_cell_measurement_reflns_used         7919
_cell_measurement_theta_min              2
_cell_measurement_theta_max             27
_cell_measurement_temperature          300
 
_exptl_crystal_description        'block' 
_exptl_crystal_colour             'blue' 
_exptl_crystal_size_min           0.060 
_exptl_crystal_size_mid           0.070 
_exptl_crystal_size_max           0.110 
 
_exptl_crystal_density_diffrn     1.545 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              984
_exptl_absorpt_coefficient_mu     1.60 
 
# Sheldrick geometric approximatio 0.89 0.91 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'SADABS (Siemens, 1996)' 
_exptl_absorpt_correction_T_min   0.80 
_exptl_absorpt_correction_T_max   0.91 
_diffrn_measurement_device_type   'Bruker Kappa Apex2' 
_diffrn_measurement_device        'Area' 
_diffrn_radiation_monochromator   'graphite' 
_diffrn_radiation_type            'Mo K\a'
_diffrn_radiation_wavelength           0.71073
_diffrn_measurement_method        ω 
 
# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection        'Apex2 (Bruker AXS, 2006)' 
_computing_cell_refinement        'Apex2 (Bruker AXS, 2006)' 
_computing_data_reduction         'SAINT (Siemens ,1995)' 
_computing_structure_solution     'USER DEFINED STRUCTURE SOLUTION' 
_computing_structure_refinement   'CRYSTALS (Betteridge et al., 2003)' 
_computing_publication_material   'CRYSTALS (Betteridge et al., 2003)' 
_computing_molecular_graphics     'CAMERON (Watkin et al., 1996)' 
 
_diffrn_standards_interval_time   . 
_diffrn_standards_interval_count  . 
_diffrn_standards_number          0 
_diffrn_standards_decay_%         ? 
 
_diffrn_ambient_temperature        300
_diffrn_reflns_number             24540 
_reflns_number_total              1894 
_diffrn_reflns_av_R_equivalents   0.061 
# Number of reflections without Friedels Law is 1894 
# Number of reflections with Friedels Law is 1894 
# Theoretical number of reflections is about 1738 
 
 
_diffrn_reflns_theta_min          1.257 
_diffrn_reflns_theta_max          28.368 
_diffrn_measured_fraction_theta_max 0.994 
 
_diffrn_reflns_theta_full         27.800 
_diffrn_measured_fraction_theta_full 0.996 
 
 
_diffrn_reflns_limit_h_min        -21 
_diffrn_reflns_limit_h_max        0 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        25 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        9 
_reflns_limit_h_min               -21 
_reflns_limit_h_max               0 
_reflns_limit_k_min               0 
_reflns_limit_k_max               25 
_reflns_limit_l_min               0 
_reflns_limit_l_max               9 
 
_oxford_diffrn_Wilson_B_factor    1.79 
_oxford_diffrn_Wilson_scale       52.81 
 
_atom_sites_solution_primary      Other  #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    difmap
 
_refine_diff_density_min          -0.58 
_refine_diff_density_max          0.63 
 
 
# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 
 
 
# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref     I>-10.0\s(I)
_refine_ls_number_reflns          1894 
_refine_ls_number_restraints      6 
_refine_ls_number_parameters      103 
_oxford_refine_ls_R_factor_ref    0.0490 
_refine_ls_wR_factor_ref          0.0823 
_refine_ls_goodness_of_fit_ref    0.9536 
_refine_ls_shift/su_max           0.0010700 
_refine_ls_shift/su_mean          0.0000494 
 
 
# The values computed with all filters except I/sigma 
_oxford_reflns_number_all         1894 
_refine_ls_R_factor_all           0.0490 
_refine_ls_wR_factor_all          0.0823 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0σ(I)
_reflns_number_gt                 1441 
_refine_ls_R_factor_gt            0.0322 
_refine_ls_wR_factor_gt           0.0762 
 
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration  '.' 
 
 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full
_refine_ls_hydrogen_treatment     constr         #undef, noref, refall,
                                                 # refxyz, refU, constr or mixed
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.04P)² + 2.30P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
# Insert your own references if required - in alphabetical order 
_publ_section_references 
; 
User-defined structure solution reference 
 
Betteridge, P.W., Carruthers, J.R., Cooper, R.I., 
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 
 
Bruker Analytical X-ray Systems, Inc., 2006. Apex2, 
Version 2 User Manual, M86-E01078, Madison, WI. 
 
Siemens Industrial Automation, Inc (1995). 
SAINT: Area-Detector Integration Software.; Madison, WI. 
 
Siemens Industrial Automation, Inc (1996). 
SADABS: Area-Detector Absorption Correction;: Madison, WI. 
 
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical 
Crystallography Laboratory, Oxford, UK. 
; 

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cu1 Cu 0.522616(10) 0.477384(10) 0.34447(5) 0.0224 1.0000 Uani S T . . . . 
C1 C 0.84646(15) 0.6929(3) 1.1740(6) 0.0558 1.0000 Uani S T . . . . 
C2 C 0.82154(12) 0.6431(2) 0.9922(5) 0.0407 1.0000 Uani S T . . . . 
C3 C 0.74565(15) 0.61975(16) 0.9072(4) 0.0381 1.0000 Uani . . . . . . 
C4 C 0.72346(13) 0.57588(15) 0.7336(3) 0.0305 1.0000 Uani . . . . . . 
C5 C 0.77738(10) 0.5548(2) 0.6456(5) 0.0300 1.0000 Uani S T . . . . 
C6 C 0.64087(13) 0.54874(14) 0.6445(3) 0.0287 1.0000 Uani . . . . . . 
C7 C 0.9508(6) 0.7617(6) 1.4133(12) 0.1130 0.5000 Uani . . . . . . 
C8 C 0.60055(13) 0.39945(13) 0.0741(7) 0.0789 1.0000 Uani S T . . . . 
O1 O 0.91557(17) 0.7126(2) 1.2447(4) 0.0949 1.0000 Uani . . . . . . 
O2 O 0.62830(10) 0.51872(13) 0.4775(3) 0.0458 1.0000 Uani . . . . . . 
O3 O 0.58975(10) 0.55683(13) 0.7448(3) 0.0472 1.0000 Uani . . . . . . 
O4 O 0.55790(7) 0.44210(7) 0.0843(3) 0.0449 1.0000 Uani DS T . . . . 
H4 H 0.5459 0.4541 -0.0224 0.0500 1.0000 Uiso DRS . . . . . 
H31 H 0.7087 0.6338 0.9680 0.0457 1.0000 Uiso R . . . . . 
H51 H 0.7630 0.5259 0.5253 0.0361 1.0000 Uiso RS . . . . . 
H71 H 1.0053 0.7680 1.4368 0.1344 0.5000 Uiso R . . . . . 
H72 H 0.9564 0.8162 1.3946 0.1344 0.5000 Uiso R . . . . . 
H73 H 0.9149 0.7344 1.5251 0.1344 0.5000 Uiso R . . . . . 
H81 H 0.6091 0.3909 -0.0625 0.0948 1.0000 Uiso RS . . . . . 
H82 H 0.5686 0.3459 0.1387 0.0948 1.0000 Uiso R . . . . . 
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.02545(17) 0.02545(17) 0.02353(19) 0.00023(7) -0.00023(7) 0.01815(17) 
C1 0.0487(16) 0.072(3) 0.055(3) -0.029(2) -0.0146(11) 0.0359(15) 
C2 0.0358(13) 0.051(2) 0.040(2) -0.0179(17) -0.0089(8) 0.0255(11) 
C3 0.0320(13) 0.0479(15) 0.0436(14) -0.0118(12) -0.0041(11) 0.0269(12) 
C4 0.0238(11) 0.0358(12) 0.0361(12) -0.0032(10) -0.0029(9) 0.0181(10) 
C5 0.0267(11) 0.0358(17) 0.0305(16) -0.0032(14) -0.0016(7) 0.0179(9) 
C6 0.0257(11) 0.0315(12) 0.0344(12) 0.0014(9) -0.0013(9) 0.0185(9) 
C7 0.122(9) 0.136(9) 0.091(6) -0.038(6) -0.040(6) 0.072(7) 
C8 0.111(4) 0.111(4) 0.067(3) -0.0059(11) 0.0059(11) 0.096(4) 
O1 0.0762(17) 0.135(3) 0.0854(17) -0.0670(18) -0.0472(15) 0.0618(18) 
O2 0.0324(9) 0.0747(14) 0.0401(10) -0.0208(9) -0.0095(8) 0.0341(10) 
O3 0.0301(9) 0.0802(14) 0.0416(10) -0.0183(10) -0.0077(8) 0.0352(10) 
O4 0.0666(14) 0.0666(14) 0.0269(12) -0.0016(5) 0.0016(5) 0.0525(16) 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 0.14720(8) 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
Cu1 . O3 12_556 1.9644(16)    yes
Cu1 . O3 2_666 1.9644(16)    yes
Cu1 . O2 11_665 1.9529(16)    yes
Cu1 . Cu1 2_666 2.5932(7)    yes
Cu1 . O2 . 1.9529(16)    yes
Cu1 . O4 . 2.123(2)    yes
C1 . O1 7_655 1.252(3)    yes
C1 . C2 . 1.489(5)    yes
C1 . O1 . 1.252(3)    yes
C2 . C3 7_655 1.388(3)    yes
C2 . C3 . 1.388(3)    yes
C3 . C4 . 1.389(3)    yes
C3 . H31 . 0.950    no
C4 . C5 . 1.392(3)    yes
C4 . C6 . 1.495(3)    yes
C5 . H51 . 0.950    no
C6 . O2 . 1.248(3)    yes
C6 . O3 . 1.248(3)    yes
C7 . H71 10_768 1.313    no
C7 . O1 . 1.420(8)    yes
C7 . H71 . 0.980    no
C7 . H72 . 0.980    no
C7 . H73 . 0.980    no
C8 . H82 11_665 0.980    no
C8 . O4 . 1.383(5)    yes
C8 . H81 . 0.980    no
C8 . H82 . 0.980    no
O4 . H4 . 0.830    no
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
O3 12_556 Cu1 . O3 2_666 88.50(13)    yes
O3 12_556 Cu1 . O2 11_665 169.01(7)    yes
O3 2_666 Cu1 . O2 11_665 89.95(9)    yes
O3 12_556 Cu1 . Cu1 2_666 83.90(5)    yes
O3 2_666 Cu1 . Cu1 2_666 83.90(5)    yes
O2 11_665 Cu1 . Cu1 2_666 85.12(5)    yes
O3 12_556 Cu1 . O2 . 89.95(9)    yes
O3 2_666 Cu1 . O2 . 169.01(7)    yes
O2 11_665 Cu1 . O2 . 89.50(12)    yes
Cu1 2_666 Cu1 . O2 . 85.12(5)    yes
O3 12_556 Cu1 . O4 . 94.79(7)    yes
O3 2_666 Cu1 . O4 . 94.79(7)    yes
O2 11_665 Cu1 . O4 . 96.18(7)    yes
Cu1 2_666 Cu1 . O4 . 178.16(7)    yes
O2 . Cu1 . O4 . 96.18(7)    yes
O1 7_655 C1 . C2 . 117.7(2)    yes
O1 7_655 C1 . O1 . 124.6(4)    yes
C2 . C1 . O1 . 117.7(2)    yes
C1 . C2 . C3 7_655 120.09(16)    yes
C1 . C2 . C3 . 120.09(16)    yes
C3 7_655 C2 . C3 . 119.8(3)    yes
C2 . C3 . C4 . 120.3(2)    yes
C2 . C3 . H31 . 119.9    no
C4 . C3 . H31 . 119.9    no
C3 . C4 . C5 . 119.8(2)    yes
C3 . C4 . C6 . 120.4(2)    yes
C5 . C4 . C6 . 119.8(2)    yes
C4 . C5 . C4 7_655 120.1(3)    yes
C4 . C5 . H51 . 120.0    no
C4 7_655 C5 . H51 . 120.0    no
C4 . C6 . O2 . 117.41(19)    yes
C4 . C6 . O3 . 117.1(2)    yes
O2 . C6 . O3 . 125.4(2)    yes
H71 10_768 C7 . O1 . 137.3    no
H71 10_768 C7 . H71 . 42.4    no
O1 . C7 . H71 . 109.3    no
H71 10_768 C7 . H72 . 110.4    no
O1 . C7 . H72 . 109.8    no
H71 . C7 . H72 . 109.5    no
H71 10_768 C7 . H73 . 69.6    no
O1 . C7 . H73 . 109.2    no
H71 . C7 . H73 . 109.5    no
H72 . C7 . H73 . 109.5    no
H82 11_665 C8 . O4 . 109.5    no
H82 11_665 C8 . H81 . 109.5    no
O4 . C8 . H81 . 109.4    no
H82 11_665 C8 . H82 . 109.5    no
O4 . C8 . H82 . 109.5    no
H81 . C8 . H82 . 109.5    no
C7 . O1 . C1 . 125.7(5)    yes
C6 . O2 . Cu1 . 122.35(15)    yes
C6 . O3 . Cu1 2_666 123.19(15)    yes
C8 . O4 . Cu1 . 125.5(3)    yes
C8 . O4 . H4 . 115.0    no
Cu1 . O4 . H4 . 119.5    no
C7 . H71 . C7 10_768 119.9    no


_iucr_refine_instruction_details_constraints
;
#
# Punched on 02/10/12 at 10:28:43
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) H   (  72,X'S) H   (  73,X'S) 
RIDE C   (   8,X'S) H   (  82,X'S) H   (  81,X'S) 
RIDE O   (   4,X'S) H   (   4,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints
;
#
# Punched on 02/10/12 at 10:28:43
#
#LIST     16                                                                    
DIST 0.84, 0.01 = O(4) TO H(4) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

#===END

data_st1004 
_audit_creation_date        "12-10-02"
_audit_creation_method CRYSTALS_ver_14.40

_publ_contact_author_name         'Stephen A. Moggach' 
_publ_contact_author_address 
; 
 Dr Stephen Moggach 
 RSE Personal Research Fellow 
 The University of Edinburgh 
 Joseph Black Building 
 West Mains Road 
 Edinburgh 
 EH9 3JJ 
; 
 
_publ_contact_author_phone        '+44(0)131 6504806' 
_publ_contact_author_email        'smoggach@staffmail.ed.ac.uk'

;
#===============================================================================

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


022_ALERT_3_B Ratio Unique / Expected Reflections (too) Low ..       0.78       
029_ALERT_3_B _diffrn_measured_fraction_theta_full Low .......       0.78 
341_ALERT_3_B Low Bond Precision on  C-C Bonds ...............       7.00 Ang. 
023_ALERT_3_C Resolution (too) Low [sin(theta)/Lambda < 0.6]..      15.72 Deg.  
088_ALERT_3_C Poor Data / Parameter Ratio ....................       6.45       
911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.558        246   
910_ALERT_3_G Missing # of FCF Reflections Below Th(Min) .....          1       
913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....         73 

The high pressure cell causes shading of a significant proportion of the
sphere of reflections. This means that the completeness is reduced and as
such the quality of the model is lower.All of the above are cause by shading 
by the pressure cell.

      
199_ALERT_1_B Check the Reported _cell_measurement_temperature        293 K     
200_ALERT_1_B Check the Reported   _diffrn_ambient_temperature        293 K  

Correct

   
301_ALERT_3_B Note: Main Residue  Disorder ...................          5 %  

C7 is disordered    
 
 
779_ALERT_4_B Suspect or Irrelevant (Bond) Angle in CIF .... #                
              H71  -C7   -H71    10.762   1.555   1.555     

Not a real bond

601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of .        265 Ang3 
041_ALERT_1_G Calc. and Reported SumFormula    Strings  Differ          ?
042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ          ?
043_ALERT_1_G Check Reported Molecular Weight ................     981.27       
044_ALERT_1_G Calculated and Reported Dx Differ ..............          ?

Structure is a porous framework with disordered solvent in the pores.
The solvent region was treated by the van der Sluis and Spek method. 
See below. This corresponds to 2 molecules of methanol per formula unit. 
F(000), M, mu, D and the given formulae have been calculated on this 
assumption.                    


045_ALERT_1_G Calculated and Reported Z Differ by ............       3.00 Ratio 

due to choice of formula unit


220_ALERT_2_G Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       3.69 Ratio 
222_ALERT_3_G Large Non-Solvent    H    Uiso(max)/Uiso(min) ..       4.25 Ratio 

This is caused by C7 which is disordered and subject to thermal motion.
Half occupied carbon refined anistropically.


241_ALERT_2_G Check High      Ueq as Compared to Neighbors for         O2     
242_ALERT_2_G Check Low       Ueq as Compared to Neighbors for        Cu1 

O2 is adjacent to the heavy atom Cu1 

    
732_ALERT_1_G Angle   Calc    117.4(5), Rep    117.4(2) ......       2.50 su-Rat
              C2   -C1   -O1      1.555   1.555   1.555                         
752_ALERT_4_G Angle   Calc      119.96, Rep    119.9(2) ......  Senseless su    
              C1   -C2   -C3      1.555   1.555   1.555

The use of restraints in the refinement mean that off diagonal terms in the
variance-covariance matrix are significant, and the diagonal approximation
used in Platon/Checkcif is badly in error.
                         
764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) .       1.06 Ratio 

No action taken
      
#===============================================================================
; 

loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000 -0.009       262        55 ' '
   2  0.667  0.333  0.463        49        22 ' '
   3  0.333  0.667  0.537        49        22 ' '
_platon_squeeze_details
;
see above for details
;
 
 
_publ_section_exptl_refinement 
; 
; 
 
_publ_section_exptl_prep 
# Brief details or a reference. Include solvent if known 
; 
? 
; 
 
#end of refcif 
_cell_length_a                    18.6631(14)
_cell_length_b                    18.6631(14)
_cell_length_c                    6.9006(5)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      2081.5(3)
 
_symmetry_cell_setting            'trigonal' 
_symmetry_space_group_name_H-M    'P -3 m 1 ' 
_symmetry_space_group_name_Hall   '-P 3 2"'
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 '-x,-y,-z'
 '-y,x-y,z'
 'y,-x+y,-z'
 '-x+y,-x,z'
 'x-y,x,-z'
 '-x+y,y,z'
 'x-y,-y,-z'
 'x,x-y,z'
 '-x,-x+y,-z'
 '-y,-x,z'
 'y,x,-z'

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source  
 Cu      0.2947   0.6374  13.3380   3.5828   7.1676   0.2470   5.6158  11.3966
   1.6735  64.8126   1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 O       0.0036   0.0026   3.0485  13.2771   2.2868   5.7011   1.5463   0.3239
   0.8670  32.9089   0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 C       0.0006   0.0007   2.3100  20.8439   1.0200  10.2075   1.5886   0.5687
   0.8650  51.6512   0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 H       0.0000   0.0000   0.4930  10.5109   0.3229  26.1257   0.1402   3.1424
   0.0408  57.7998   0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 
 
_cell_formula_units_Z                    2

# Given Formula = C30 H21 Cu3 O21 
# Dc =      1.45 Fooo =    966.00 Mu =     15.93 M =    151.35
# Found Formula = C33 H30 Cu3 O21 
# Dc =      1.52 FOOO =    966.00 Mu =     15.97 M =    158.87

_chemical_formula_sum             'C35 H38 Cu3 O23'
_chemical_formula_moiety          'C33 H30 Cu3 O21.2CH3OH'
_chemical_compound_source                ?
_chemical_formula_weight            981.27
 
 
_cell_measurement_reflns_used         2252
_cell_measurement_theta_min              2
_cell_measurement_theta_max             15
_cell_measurement_temperature          293
 
_exptl_crystal_description        'block' 
_exptl_crystal_colour             'blue' 
_exptl_crystal_size_min           0.100 
_exptl_crystal_size_mid           0.200 
_exptl_crystal_size_max           0.200 
 
_exptl_crystal_density_diffrn     1.566
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              1002 
_exptl_absorpt_coefficient_mu     0.525
 
# Sheldrick geometric approximatio 0.73 0.85 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'SADABS (Siemens, 1996)' 
_exptl_absorpt_correction_T_min   0.44 
_exptl_absorpt_correction_T_max   0.85 
_diffrn_measurement_device_type   'Rigaku Saturn 724+' 
_diffrn_measurement_device        'Area' 
_diffrn_radiation_monochromator   'graphite' 
_diffrn_radiation_type            'synchrotron'
_diffrn_radiation_wavelength           0.48590
_diffrn_measurement_method        ω 
 
# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection        'Gemini, (Oxford Diffraction, 2006)' 
_computing_cell_refinement        'CrysAlis, (Oxford Diffraction, 2002)' 
_computing_data_reduction         'Apex2 (Bruker AXS, 2006)' 
_computing_structure_solution     'USER DEFINED STRUCTURE SOLUTION' 
_computing_structure_refinement   'CRYSTALS (Betteridge et al., 2003)' 
_computing_publication_material   'CRYSTALS (Betteridge et al., 2003)' 
_computing_molecular_graphics     'CAMERON (Watkin et al., 1996)' 
 
_diffrn_standards_interval_time   . 
_diffrn_standards_interval_count  . 
_diffrn_standards_number          0 
_diffrn_standards_decay_%         ? 
 
_diffrn_ambient_temperature        293
_diffrn_reflns_number             11549 
_reflns_number_total              876 
_diffrn_reflns_av_R_equivalents   0.0928 
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 876 
# Theoretical number of reflections is about 2017 
 
 
_diffrn_reflns_theta_min          1.492 
_diffrn_reflns_theta_max          15.723 
_diffrn_measured_fraction_theta_max 0.780 
 
_diffrn_reflns_theta_full         15.408 
_diffrn_measured_fraction_theta_full 0.781 
 
 
_diffrn_reflns_limit_h_min        -16 
_diffrn_reflns_limit_h_max        0 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        20 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        7 
_reflns_limit_h_min               -16 
_reflns_limit_h_max               0 
_reflns_limit_k_min               0 
_reflns_limit_k_max               20 
_reflns_limit_l_min               0 
_reflns_limit_l_max               7 
 
_oxford_diffrn_Wilson_B_factor    0.00 
_oxford_diffrn_Wilson_scale       0.00 
 
_atom_sites_solution_primary      Other  #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    difmap
 
_refine_diff_density_min          -0.45 
_refine_diff_density_max          0.63 
 
 
# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 
 
 
# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref     I>2.0\s(I)
_refine_ls_number_reflns          664 
_refine_ls_number_restraints      132 
_refine_ls_number_parameters      103 
_oxford_refine_ls_R_factor_ref    0.0407 
_refine_ls_wR_factor_ref          0.0467 
_refine_ls_goodness_of_fit_ref    1.1519 
_refine_ls_shift/su_max           0.0008504 
_refine_ls_shift/su_mean          0.0000396 
 
 
# The values computed with all filters except I/sigma 
_oxford_reflns_number_all         871 
_refine_ls_R_factor_all           0.0620 
_refine_ls_wR_factor_all          0.0742 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0σ(I)
_reflns_number_gt                 664 
_refine_ls_R_factor_gt            0.0407 
_refine_ls_wR_factor_gt           0.0467 
 
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration  '.' 
 
 
_refine_ls_structure_factor_coef  F 
_refine_ls_matrix_type            full
_refine_ls_hydrogen_treatment     constr         #undef, noref, refall,
                                                 # refxyz, refU, constr or mixed
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.288 0.159 0.898E-01 
;
# Insert your own references if required - in alphabetical order 
_publ_section_references 
; 
User-defined structure solution reference 
 
Betteridge, P.W., Carruthers, J.R., Cooper, R.I., 
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 
 
Bruker Analytical X-ray Systems, Inc., 2006. Apex2, 
Version 2 User Manual, M86-E01078, Madison, WI. 
 
Oxford Diffraction, (2010). CrysAlisPro. 
 
Oxford Diffraction, (2006). Gemini User Manual. 
 
Prince, E. 
Mathematical Techniques in Crystallography 
and Materials Science 
Springer-Verlag, New York, 1982. 
 
Watkin D.J. (1994). 
Acta Cryst, A50, 411-437. 
 
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical 
Crystallography Laboratory, Oxford, UK. 
; 

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cu1 Cu 0.52295(2) 0.04591(5) -0.34563(11) 0.0214 1.0000 Uani S T . . . . 
C1 C 0.8409(3) 0.1591(3) -1.1914(9) 0.0472 1.0000 Uani DS TU . . . . 
C2 C 0.8172(2) 0.1828(2) -1.0057(8) 0.0327 1.0000 Uani DS TU . . . . 
C3 C 0.7428(3) 0.1284(3) -0.9167(6) 0.0320 1.0000 Uani D U . . . . 
C4 C 0.7229(2) 0.1485(3) -0.7392(5) 0.0264 1.0000 Uani D U . . . . 
C5 C 0.7785(2) 0.2215(2) -0.6478(8) 0.0253 1.0000 Uani DS TU . . . . 
C6 C 0.6411(2) 0.0915(3) -0.6463(6) 0.0254 1.0000 Uani D U . . . . 
C7 C 0.9471(9) 0.1974(9) -1.4282(19) 0.0930 0.5000 Uani D U . . . . 
C8 C 0.6002(2) 0.2005(4) -0.0722(14) 0.0718 1.0000 Uani DS TU . . . . 
O1 O 0.9097(3) 0.2095(3) -1.2629(7) 0.0848 1.0000 Uani D U . . . . 
O2 O 0.6287(2) 0.1103(2) -0.4801(5) 0.0454 1.0000 Uani D U . . . . 
O3 O 0.5889(2) 0.0315(2) -0.7436(5) 0.0477 1.0000 Uani D U . . . . 
O4 O 0.55766(15) 0.1153(3) -0.0833(6) 0.0421 1.0000 Uani DS TU . . . . 
H4 H 0.5375 0.0750 -0.0108 0.0500 1.0000 Uiso DRS . . . . . 
H81 H 0.6084 0.2168 0.0616 0.0915 1.0000 Uiso RS . . . . . 
H82 H 0.6530 0.2219 -0.1348 0.0915 1.0000 Uiso R . . . . . 
H71 H 1.0002 0.2455 -1.4505 0.1223 0.5000 Uiso R . . . . . 
H72 H 0.9535 0.1498 -1.4137 0.1223 0.5000 Uiso R . . . . . 
H73 H 0.9114 0.1894 -1.5362 0.1223 0.5000 Uiso R . . . . . 
H31 H 0.7061 0.0787 -0.9766 0.0380 1.0000 Uiso R . . . . . 
H51 H 0.7670 0.2330 -0.5244 0.0288 1.0000 Uiso RS . . . . . 
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0237(4) 0.0144(5) 0.0230(4) 0.0015(3) 0.00073(17) 0.0072(2) 
C1 0.051(2) 0.051(2) 0.040(4) -0.0076(16) 0.0076(16) 0.025(3) 
C2 0.027(2) 0.027(2) 0.039(3) -0.0041(14) 0.0041(14) 0.010(2) 
C3 0.026(2) 0.020(3) 0.041(2) -0.006(2) 0.0014(18) 0.0042(19) 
C4 0.020(2) 0.024(2) 0.033(2) 0.0009(17) -0.0009(16) 0.0095(16) 
C5 0.0250(19) 0.0250(19) 0.025(3) 0.0003(13) -0.0003(13) 0.012(2) 
C6 0.019(2) 0.024(2) 0.033(2) -0.0007(16) -0.0012(15) 0.0109(15) 
C7 0.117(13) 0.089(13) 0.077(9) 0.012(9) 0.059(9) 0.054(11) 
C8 0.094(7) 0.032(3) 0.069(6) -0.011(5) -0.005(2) 0.0162(14) 
O1 0.085(4) 0.077(4) 0.077(3) 0.002(3) 0.051(3) 0.029(3) 
O2 0.026(2) 0.045(2) 0.0378(17) -0.0120(17) 0.0056(16) -0.0031(17) 
O3 0.025(2) 0.046(2) 0.0405(19) -0.0120(16) 0.0091(15) -0.0058(16) 
O4 0.060(3) 0.031(2) 0.026(2) -0.002(2) -0.0008(11) 0.0153(12) 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 0.1270(5) 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
Cu1 . O2 7_655 1.957(3)    yes
Cu1 . O3 8_554 1.951(3)    yes
Cu1 . O3 2_654 1.951(3)    yes
Cu1 . O2 . 1.957(3)    yes
Cu1 . O4 . 2.130(4)    yes
C1 . O1 11_665 1.253(4)    yes
C1 . C2 . 1.493(6)    yes
C1 . O1 . 1.253(4)    yes
C2 . C3 11_665 1.388(4)    yes
C2 . C3 . 1.388(4)    yes
C3 . C4 . 1.385(5)    yes
C3 . H31 . 0.930    no
C4 . C5 . 1.385(4)    yes
C4 . C6 . 1.499(5)    yes
C5 . H51 . 0.930    no
C6 . O2 . 1.254(5)    yes
C6 . O3 . 1.251(5)    yes
C7 . H71 10_762 1.260    no
C7 . O1 . 1.413(7)    yes
C7 . H71 . 0.960    no
C7 . H72 . 0.960    no
C7 . H73 . 0.960    no
C8 . H82 7_655 0.960    no
C8 . O4 . 1.378(7)    yes
C8 . H81 . 0.960    no
C8 . H82 . 0.960    no
O4 . H4 . 0.822    no
H71 . H71 10_762 0.684    no
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
O2 7_655 Cu1 . O3 8_554 168.96(13)    yes
O2 7_655 Cu1 . O3 2_654 89.99(18)    yes
O3 8_554 Cu1 . O3 2_654 88.8(3)    yes
O2 7_655 Cu1 . O2 . 89.1(3)    yes
O3 8_554 Cu1 . O2 . 89.99(18)    yes
O3 2_654 Cu1 . O2 . 168.96(13)    yes
O2 7_655 Cu1 . O4 . 97.06(13)    yes
O3 8_554 Cu1 . O4 . 93.97(13)    yes
O3 2_654 Cu1 . O4 . 93.97(13)    yes
O2 . Cu1 . O4 . 97.06(13)    yes
O1 11_665 C1 . C2 . 117.4(2)    yes
O1 11_665 C1 . O1 . 125.2(5)    yes
C2 . C1 . O1 . 117.4(2)    yes
C1 . C2 . C3 11_665 119.9(2)    yes
C1 . C2 . C3 . 119.9(2)    yes
C3 11_665 C2 . C3 . 120.0(4)    yes
C2 . C3 . C4 . 119.9(3)    yes
C2 . C3 . H31 . 120.1    no
C4 . C3 . H31 . 120.0    no
C3 . C4 . C5 . 119.9(3)    yes
C3 . C4 . C6 . 120.1(3)    yes
C5 . C4 . C6 . 120.0(3)    yes
C4 11_665 C5 . C4 . 120.2(4)    yes
C4 11_665 C5 . H51 . 119.9    no
C4 . C5 . H51 . 119.9    no
C4 . C6 . O2 . 117.3(3)    yes
C4 . C6 . O3 . 117.8(3)    yes
O2 . C6 . O3 . 124.8(3)    yes
H71 10_762 C7 . O1 . 134.1    no
H71 10_762 C7 . H71 . 32.4    no
O1 . C7 . H71 . 110.0    no
H71 10_762 C7 . H72 . 108.1    no
O1 . C7 . H72 . 111.3    no
H71 . C7 . H72 . 109.5    no
H71 10_762 C7 . H73 . 80.2    no
O1 . C7 . H73 . 107.1    no
H71 . C7 . H73 . 109.5    no
H72 . C7 . H73 . 109.5    no
H82 7_655 C8 . O4 . 109.6    no
H82 7_655 C8 . H81 . 109.5    no
O4 . C8 . H81 . 109.1    no
H82 7_655 C8 . H82 . 109.5    no
O4 . C8 . H82 . 109.6    no
H81 . C8 . H82 . 109.5    no
C7 . O1 . C1 . 127.0(6)    yes
C6 . O2 . Cu1 . 122.2(3)    yes
C6 . O3 . Cu1 8_554 124.0(3)    yes
C8 . O4 . Cu1 . 125.0(5)    yes
C8 . O4 . H4 . 139.3    no
Cu1 . O4 . H4 . 95.7    no
H71 10_762 H71 . C7 . 98.7    no
H71 10_762 H71 . C7 10_762 48.8    no
C7 . H71 . C7 10_762 125.3    no


_iucr_refine_instruction_details_constraints
;
#
# Punched on 02/10/12 at 14:35:19
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) H   (  72,X'S) H   (  73,X'S) 
RIDE C   (   8,X'S) H   (  82,X'S) H   (  81,X'S) 
RIDE O   (   4,X'S) H   (   4,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints
;
#
# Punched on 02/10/12 at 14:35:19
#
#LIST     16                                                                    
DIST 0.82, 0.01 = O(4) TO H(4) 
DIST   1.489,.01= C(1) TO C(2) 
DIST   1.252,.01= C(1) TO O(1) 
DIST   1.252,.01= C(1) TO O(1,6,1,1,1) 
DIST   1.388,.01= C(2) TO C(3) 
DIST   1.388,.01= C(2) TO C(3,6,1,1,1) 
DIST   1.389,.01= C(3) TO C(4) 
DIST   1.392,.01= C(4) TO C(5) 
DIST   1.495,.01= C(4) TO C(6) 
DIST   1.248,.01= C(6) TO O(2) 
DIST   1.248,.01= C(6) TO O(3) 
DIST   1.420,.01= C(7) TO O(1) 
DIST   1.383,.01= C(8) TO O(4) 
ANGL 118,1= O(1) TO C(1) TO C(2) 
ANGL 118,1= O(1,6,1,1,1) TO C(1) TO C(2) 
ANGL 125,1= O(1,6,1,1,1) TO C(1) TO O(1) 
ANGL 120,1= C(3) TO C(2) TO C(1) 
ANGL 120,1= C(3,6,1,1,1) TO C(2) TO C(1) 
ANGL 120,1= C(3,6,1,1,1) TO C(2) TO C(3) 
ANGL 120,1= C(4) TO C(3) TO C(2) 
ANGL 120,1= C(5) TO C(4) TO C(3) 
ANGL 120,1= C(6) TO C(4) TO C(3) 
ANGL 120,1= C(6) TO C(4) TO C(5) 
ANGL 120,1= C(4,6,1,1,1) TO C(5) TO C(4) 
ANGL 117,1= O(2) TO C(6) TO C(4) 
ANGL 117,1= O(3) TO C(6) TO C(4) 
ANGL 125,1= O(3) TO C(6) TO O(2) 
ANGL 126,1= C(7) TO O(1) TO C(1) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = C(1) TO O(1,6,1,1,1) 
VIBR .0, 0.00200 = C(1) TO C(2) 
VIBR .0, 0.00200 = C(1) TO O(1) 
VIBR .0, 0.00500 = C(2) TO O(1,6,1,1,1) 
VIBR .0, 0.00500 = O(1) TO O(1,6,1,1,1) 
VIBR .0, 0.00500 = O(1) TO C(2) 
VIBR .0, 0.00200 = C(2) TO C(3,6,1,1,1) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00500 = C(3,6,1,1,1) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(3,6,1,1,1) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00200 = C(4) TO C(5) 
VIBR .0, 0.00200 = C(4) TO C(6) 
VIBR .0, 0.00500 = C(5) TO C(3) 
VIBR .0, 0.00500 = C(6) TO C(3) 
VIBR .0, 0.00500 = C(6) TO C(5) 
VIBR .0, 0.00500 = C(4,6,1,1,1) TO C(4) 
VIBR .0, 0.00200 = C(6) TO O(2) 
VIBR .0, 0.00200 = C(6) TO O(3) 
VIBR .0, 0.00500 = O(2) TO C(4) 
VIBR .0, 0.00500 = O(3) TO C(4) 
VIBR .0, 0.00500 = O(3) TO O(2) 
VIBR .0, 0.00200 = C(7) TO O(1) 
VIBR .0, 0.00200 = C(8) TO O(4) 
VIBR .0, 0.00500 = C(1) TO C(7) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = C(1) TO O(1,6,1,1,1) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.04000 = C(1) TO O(1) 
U(IJ) .0, 0.04000 = C(2) TO C(3,6,1,1,1) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(4) TO C(5) 
U(IJ) .0, 0.04000 = C(4) TO C(6) 
U(IJ) .0, 0.08000 = C(6) TO O(2) 
U(IJ) .0, 0.08000 = C(6) TO O(3) 
U(IJ) .0, 0.08000 = C(7) TO O(1) 
U(IJ) .0, 0.08000 = C(8) TO O(4) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
  -1  10   2  x   .
   0  12   0  x   .
  -1   3   0  x   .
   0   3   1  x   .
  -1   2   0  x   .

#===END

data_st1005
_audit_creation_date        "12-10-02"
_audit_creation_method CRYSTALS_ver_14.40


_publ_contact_author_name         'Stephen A. Moggach' 
_publ_contact_author_address 
; 
 Dr Stephen Moggach 
 RSE Personal Research Fellow 
 The University of Edinburgh 
 Joseph Black Building 
 West Mains Road 
 Edinburgh 
 EH9 3JJ 
; 
 
_publ_contact_author_phone        '+44(0)131 6504806' 
_publ_contact_author_email        'smoggach@staffmail.ed.ac.uk' 

;
#===============================================================================

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

027_ALERT_3_B _diffrn_reflns_theta_full (too) Low ............      12.09 Deg.  
029_ALERT_3_B _diffrn_measured_fraction_theta_full Low .......       0.94  
341_ALERT_3_B Low Bond Precision on  C-C Bonds ...............      10.00 Ang. 
023_ALERT_3_C Resolution (too) Low [sin(theta)/Lambda < 0.6]..      15.70 Deg.  
088_ALERT_3_C Poor Data / Parameter Ratio ....................       7.50
911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.557         74 
913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....         13 
022_ALERT_3_G Ratio Unique / Expected Reflections (too) Low ..       0.93 
 

The high pressure cell causes shading of a significant proportion of the
sphere of reflections. This means that the completeness is reduced and as
such the quality of the model is lower.All of the above are cause by shading 
by the pressure cell.


601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of .        270 Ang3
043_ALERT_1_B Check Reported Molecular Weight ................    1113.43       
044_ALERT_1_B Calculated and Reported Dx Differ ..............          ?
041_ALERT_1_G Calc. and Reported SumFormula    Strings  Differ          ?
042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ          ?

Structure is a porous framework with disordered solvent in the pores.
The solvent region was treated by the van der Sluis and Spek method. 
See below. This corresponds to 5 molecules of methanol per formula unit. 
F(000), M, mu, D and the given formulae have been calculated on this 
assumption.


199_ALERT_1_B Check the Reported _cell_measurement_temperature        293 K     
200_ALERT_1_B Check the Reported   _diffrn_ambient_temperature        293 K  

correct

   
301_ALERT_3_B Note: Main Residue  Disorder ...................          5 %

C7 is disordered        
 

779_ALERT_4_B Suspect or Irrelevant (Bond) Angle in CIF .... #                
              H71  -C7   -H71    10.762   1.555   1.555  

not a real bond                       

       
220_ALERT_2_C Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       4.57 Ratio
242_ALERT_2_G Check Low       Ueq as Compared to Neighbors for         C6
222_ALERT_3_G Large Non-Solvent    H    Uiso(max)/Uiso(min) ..       4.51 Ratio 
250_ALERT_2_G Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.01 

this is caused by C7 which is disordered and subject to thermal motion.
Half occupied carbon refined anistropically. 


241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         O2     
241_ALERT_2_G Check High      Ueq as Compared to Neighbors for         O1     
242_ALERT_2_G Check Low       Ueq as Compared to Neighbors for        Cu1     
242_ALERT_2_G Check Low       Ueq as Compared to Neighbors for         C1     

Cu1 is a heavy atom
      

045_ALERT_1_G Calculated and Reported Z Differ by ............       3.00 Ratio 


due to choice of formula unit
     
      
731_ALERT_1_G Bond    Calc   1.254(11), Rep    1.255(5) ......          2 su-Rat
              C1   -O1      1.555  11.665                                       
731_ALERT_1_G Bond    Calc   1.254(12), Rep    1.255(5) ......          2 su-Rat
              C1   -O1      1.555   1.555                                       
731_ALERT_1_G Bond    Calc   1.384(11), Rep    1.384(5) ......          2 su-Rat
              C2   -C3      1.555   1.555                                       
732_ALERT_1_G Angle   Calc    117.3(7), Rep    117.4(3) ......       2.33 su-Rat
              C2   -C1   -O1      1.555   1.555   1.555            

The use of restraints in the refinement mean that off diagonal terms in the
variance-covariance matrix are significant, and the diagonal approximation
used in Platon/Checkcif is badly in error.

             
764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) .       1.06 Ratio 

no action taken
     
#===============================================================================
;

loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000 -0.008       265       159 ' '
   2  0.667  0.333  0.464        43        21 ' '
   3  0.333  0.667  0.536        43        21 ' '
_platon_squeeze_details
;
see above for details
;
 
 
_publ_section_exptl_refinement 
; 
; 
 
_publ_section_exptl_prep 
# Brief details or a reference. Include solvent if known 
; 
? 
; 
 
#end of refcif 
_cell_length_a                    18.5495(13)
_cell_length_b                    18.5495(13)
_cell_length_c                    6.8063(5)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      2028.2(3)
 
_symmetry_cell_setting            'trigonal' 
_symmetry_space_group_name_H-M    'P -3 m 1 ' 
_symmetry_space_group_name_Hall   '-P 3 2' 
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 '-x,-y,-z'
 '-y,x-y,z'
 'y,-x+y,-z'
 '-x+y,-x,z'
 'x-y,x,-z'
 '-x+y,y,z'
 'x-y,-y,-z'
 'x,x-y,z'
 '-x,-x+y,-z'
 '-y,-x,z'
 'y,x,-z'

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source  
 Cu      0.2947   0.6374  13.3380   3.5828   7.1676   0.2470   5.6158  11.3966
   1.6735  64.8126   1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 O       0.0036   0.0026   3.0485  13.2771   2.2868   5.7011   1.5463   0.3239
   0.8670  32.9089   0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 C       0.0006   0.0007   2.3100  20.8439   1.0200  10.2075   1.5886   0.5687
   0.8650  51.6512   0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 H       0.0000   0.0000   0.4930  10.5109   0.3229  26.1257   0.1402   3.1424
   0.0408  57.7998   0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 
 
_cell_formula_units_Z                    2

# Given Formula = C15 H10.50 Cu1.50 O10.50 
# Dc =      0.74 Fooo =    966.00 Mu =      8.18 M =     75.68
# Found Formula = C33 H30 Cu3 O21 
# Dc =      1.56 FOOO =    966.00 Mu =     16.39 M =    158.87

_chemical_formula_sum             'C38 H50 Cu3 O26'
_chemical_formula_moiety          'C33 H30 Cu3 O21.5CH3OH'
_chemical_compound_source                ?
_chemical_formula_weight            1113.43
 
 
_cell_measurement_reflns_used         3271
_cell_measurement_theta_min              2
_cell_measurement_theta_max             15
_cell_measurement_temperature          293
 
_exptl_crystal_description        'block' 
_exptl_crystal_colour             'blue' 
_exptl_crystal_size_min           0.100 
_exptl_crystal_size_mid           0.200 
_exptl_crystal_size_max           0.200 
 
_exptl_crystal_density_diffrn     1.823 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              1146 
_exptl_absorpt_coefficient_mu     0.542 
 
# Sheldrick geometric approximatio 0.72 0.85 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'SADABS (Siemens, 1996)' 
_exptl_absorpt_correction_T_min   0.45 
_exptl_absorpt_correction_T_max   0.85 
_diffrn_measurement_device_type   'Rigaku Saturn 724+' 
_diffrn_measurement_device        'Area' 
_diffrn_radiation_monochromator   'graphite' 
_diffrn_radiation_type            'synchrotron'
_diffrn_radiation_wavelength           0.48590
_diffrn_measurement_method        ω 
 
# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection        'Gemini, (Oxford Diffraction, 2006)' 
_computing_cell_refinement        'CrysAlis, (Oxford Diffraction, 2002)' 
_computing_data_reduction         'Apex2 (Bruker AXS, 2006)' 
_computing_structure_solution     'USER DEFINED STRUCTURE SOLUTION' 
_computing_structure_refinement   'CRYSTALS (Betteridge et al., 2003)' 
_computing_publication_material   'CRYSTALS (Betteridge et al., 2003)' 
_computing_molecular_graphics     'CAMERON (Watkin et al., 1996)' 
 
_diffrn_standards_interval_time   . 
_diffrn_standards_interval_count  . 
_diffrn_standards_number          0 
_diffrn_standards_decay_%         ? 
 
_diffrn_ambient_temperature        293
_diffrn_reflns_number             7228 
_reflns_number_total              1017 
_diffrn_reflns_av_R_equivalents   0.1094 
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 1017 
# Theoretical number of reflections is about 1942 
 
 
_diffrn_reflns_theta_min          0.867 
_diffrn_reflns_theta_max          15.703 
_diffrn_measured_fraction_theta_max 0.932 
 
_diffrn_reflns_theta_full         12.091 
_diffrn_measured_fraction_theta_full 0.936 
 
 
_diffrn_reflns_limit_h_min        -16 
_diffrn_reflns_limit_h_max        0 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        20 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        7 
_reflns_limit_h_min               -16 
_reflns_limit_h_max               0 
_reflns_limit_k_min               0 
_reflns_limit_k_max               20 
_reflns_limit_l_min               0 
_reflns_limit_l_max               7 
 
_oxford_diffrn_Wilson_B_factor    0.00 
_oxford_diffrn_Wilson_scale       0.00 
 
_atom_sites_solution_primary      Other  #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    difmap
 
_refine_diff_density_min          -1.05 
_refine_diff_density_max          0.98 
 
 
# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 
 
 
# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref     I>2.0\s(I)
_refine_ls_number_reflns          773 
_refine_ls_number_restraints      132 
_refine_ls_number_parameters      103 
_oxford_refine_ls_R_factor_ref    0.0673 
_refine_ls_wR_factor_ref          0.0925 
_refine_ls_goodness_of_fit_ref    1.2169 
_refine_ls_shift/su_max           0.0024646 
_refine_ls_shift/su_mean          0.0000353 
 
 
# The values computed with all filters except I/sigma 
_oxford_reflns_number_all         1003 
_refine_ls_R_factor_all           0.0912 
_refine_ls_wR_factor_all          0.1138 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0σ(I)
_reflns_number_gt                 773 
_refine_ls_R_factor_gt            0.0673 
_refine_ls_wR_factor_gt           0.0925 
 
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration  '.' 
 
 
_refine_ls_structure_factor_coef  F 
_refine_ls_matrix_type            full
_refine_ls_hydrogen_treatment     constr         #undef, noref, refall,
                                                 # refxyz, refU, constr or mixed
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.769 0.624 0.434 
;
# Insert your own references if required - in alphabetical order 
_publ_section_references 
; 
User-defined structure solution reference 
 
Betteridge, P.W., Carruthers, J.R., Cooper, R.I., 
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 
 
Bruker Analytical X-ray Systems, Inc., 2006. Apex2, 
Version 2 User Manual, M86-E01078, Madison, WI. 
 
Oxford Diffraction, (2010). CrysAlisPro. 
 
Oxford Diffraction, (2006). Gemini User Manual. 
 
Prince, E. 
Mathematical Techniques in Crystallography 
and Materials Science 
Springer-Verlag, New York, 1982. 
 
Watkin D.J. (1994). 
Acta Cryst, A50, 411-437. 
 
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical 
Crystallography Laboratory, Oxford, UK. 
; 

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cu1 Cu 0.52343(4) 0.04686(7) -0.34482(19) 0.0211 1.0000 Uani S T . . . . 
C1 C 0.8382(4) 0.1618(4) -1.2131(13) 0.0434 1.0000 Uani DS TU . . . . 
C2 C 0.8159(4) 0.1841(4) -1.0206(12) 0.0333 1.0000 Uani DS TU . . . . 
C3 C 0.7410(4) 0.1300(4) -0.9309(10) 0.0335 1.0000 Uani D U . . . . 
C4 C 0.7213(3) 0.1495(4) -0.7492(8) 0.0230 1.0000 Uani D U . . . . 
C5 C 0.7778(3) 0.2222(3) -0.6551(12) 0.0214 1.0000 Uani DS TU . . . . 
C6 C 0.6404(4) 0.0911(4) -0.6520(8) 0.0244 1.0000 Uani D U . . . . 
C7 C 0.9470(15) 0.1999(14) -1.450(3) 0.0974 0.5000 Uani D U . . . . 
C8 C 0.6019(3) 0.2038(6) -0.078(2) 0.0677 1.0000 Uani DS TU . . . . 
O1 O 0.9075(5) 0.2126(5) -1.2856(12) 0.0983 1.0000 Uani D U . . . . 
O2 O 0.6281(3) 0.1102(4) -0.4834(9) 0.0541 1.0000 Uani D U . . . . 
O3 O 0.5881(3) 0.0298(4) -0.7495(8) 0.0453 1.0000 Uani D U . . . . 
O4 O 0.5587(2) 0.1174(4) -0.0842(11) 0.0366 1.0000 Uani DS TU . . . . 
H4 H 0.5384 0.0768 -0.0112 0.0500 1.0000 Uiso DRS . . . . . 
H81 H 0.6089 0.2177 0.0595 0.0727 1.0000 Uiso RS . . . . . 
H82 H 0.6555 0.2266 -0.1389 0.0727 1.0000 Uiso R . . . . . 
H71 H 0.9996 0.2489 -1.4751 0.1187 0.5000 Uiso R . . . . . 
H72 H 0.9557 0.1541 -1.4215 0.1187 0.5000 Uiso R . . . . . 
H73 H 0.9119 0.1870 -1.5634 0.1187 0.5000 Uiso R . . . . . 
H31 H 0.7034 0.0807 -0.9931 0.0393 1.0000 Uiso R . . . . . 
H51 H 0.7661 0.2339 -0.5299 0.0263 1.0000 Uiso RS . . . . . 
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0226(7) 0.0095(8) 0.0268(8) 0.0038(5) 0.0019(3) 0.0048(4) 
C1 0.051(4) 0.051(4) 0.046(6) -0.008(2) 0.008(2) 0.040(4) 
C2 0.031(3) 0.031(3) 0.034(5) -0.005(2) 0.005(2) 0.012(3) 
C3 0.031(4) 0.022(4) 0.039(4) -0.007(3) 0.003(3) 0.007(3) 
C4 0.017(3) 0.021(3) 0.028(3) 0.002(2) -0.003(2) 0.007(2) 
C5 0.019(3) 0.019(3) 0.025(5) 0.000(2) 0.000(2) 0.010(3) 
C6 0.021(3) 0.016(3) 0.031(3) 0.004(2) -0.002(2) 0.006(2) 
C7 0.106(17) 0.12(2) 0.075(14) 0.024(13) 0.059(12) 0.067(17) 
C8 0.088(11) 0.025(4) 0.069(10) -0.003(7) -0.001(4) 0.0125(19) 
O1 0.101(7) 0.098(7) 0.090(6) 0.016(5) 0.068(5) 0.046(5) 
O2 0.023(3) 0.053(4) 0.051(3) -0.016(3) 0.016(3) -0.008(3) 
O3 0.024(3) 0.039(4) 0.043(3) -0.014(3) 0.011(3) -0.007(2) 
O4 0.041(4) 0.024(4) 0.039(5) 0.009(4) 0.0046(19) 0.0120(18) 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 0.1205(9) 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
Cu1 . O3 2_654 1.942(5)    yes
Cu1 . O3 8_554 1.942(5)    yes
Cu1 . O2 7_655 1.939(5)    yes
Cu1 . O2 . 1.939(5)    yes
Cu1 . O4 . 2.105(8)    yes
C1 . O1 11_665 1.255(5)    yes
C1 . C2 . 1.492(7)    yes
C1 . O1 . 1.255(5)    yes
C2 . C3 11_665 1.384(5)    yes
C2 . C3 . 1.384(5)    yes
C3 . C4 . 1.388(6)    yes
C3 . H31 . 0.930    no
C4 . C5 . 1.384(6)    yes
C4 . C6 . 1.496(6)    yes
C5 . H51 . 0.930    no
C6 . O2 . 1.255(6)    yes
C6 . O3 . 1.254(6)    yes
C7 . H71 10_762 1.084    no
C7 . O1 . 1.419(9)    yes
C7 . H71 . 0.960    no
C7 . H72 . 0.960    no
C7 . H73 . 0.960    no
C8 . H82 7_655 0.960    no
C8 . O4 . 1.389(8)    yes
C8 . H81 . 0.960    no
C8 . H82 . 0.960    no
O4 . H4 . 0.820    no
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
O3 2_654 Cu1 . O3 8_554 88.8(4)    yes
O3 2_654 Cu1 . O2 7_655 90.3(3)    yes
O3 8_554 Cu1 . O2 7_655 169.1(2)    yes
O3 2_654 Cu1 . O2 . 169.1(2)    yes
O3 8_554 Cu1 . O2 . 90.3(3)    yes
O2 7_655 Cu1 . O2 . 88.6(5)    yes
O3 2_654 Cu1 . O4 . 93.6(2)    yes
O3 8_554 Cu1 . O4 . 93.6(2)    yes
O2 7_655 Cu1 . O4 . 97.3(2)    yes
O2 . Cu1 . O4 . 97.3(2)    yes
O1 11_665 C1 . C2 . 117.4(3)    yes
O1 11_665 C1 . O1 . 125.2(6)    yes
C2 . C1 . O1 . 117.4(3)    yes
C1 . C2 . C3 11_665 120.2(3)    yes
C1 . C2 . C3 . 120.2(3)    yes
C3 11_665 C2 . C3 . 119.6(5)    yes
C2 . C3 . C4 . 120.3(4)    yes
C2 . C3 . H31 . 120.0    no
C4 . C3 . H31 . 119.7    no
C3 . C4 . C5 . 119.8(4)    yes
C3 . C4 . C6 . 120.4(4)    yes
C5 . C4 . C6 . 119.8(4)    yes
C4 . C5 . C4 11_665 120.0(5)    yes
C4 . C5 . H51 . 120.0    no
C4 11_665 C5 . H51 . 120.0    no
C4 . C6 . O2 . 117.3(4)    yes
C4 . C6 . O3 . 117.6(4)    yes
O2 . C6 . O3 . 125.0(5)    yes
H71 10_762 C7 . O1 . 124.1    no
H71 10_762 C7 . H71 . 17.9    no
O1 . C7 . H71 . 110.4    no
H71 10_762 C7 . H72 . 110.9    no
O1 . C7 . H72 . 108.5    no
H71 . C7 . H72 . 109.5    no
H71 10_762 C7 . H73 . 92.9    no
O1 . C7 . H73 . 109.5    no
H71 . C7 . H73 . 109.5    no
H72 . C7 . H73 . 109.5    no
H82 7_655 C8 . O4 . 111.5    no
H82 7_655 C8 . H81 . 109.5    no
O4 . C8 . H81 . 105.3    no
H82 7_655 C8 . H82 . 109.5    no
O4 . C8 . H82 . 111.5    no
H81 . C8 . H82 . 109.5    no
C7 . O1 . C1 . 127.3(8)    yes
C6 . O2 . Cu1 . 122.8(4)    yes
C6 . O3 . Cu1 2_654 123.1(4)    yes
C8 . O4 . Cu1 . 124.4(9)    yes
C8 . O4 . H4 . 140.9    no
Cu1 . O4 . H4 . 94.7    no
C7 10_762 H71 . C7 . 127.6    no


_iucr_refine_instruction_details_constraints
;
#
# Punched on 02/10/12 at 14:34:04
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   8,X'S) H   (  82,X'S) H   (  81,X'S) 
RIDE O   (   4,X'S) H   (   4,X'S) 
RIDE C   (   7,X'S) H   (  72,X'S) H   (  73,X'S) H   (  71,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints
;
#
# Punched on 02/10/12 at 14:34:04
#
#LIST     16                                                                    
DIST 0.82, 0.01 = O(4) TO H(4) 
DIST   1.489,.01= C(1) TO C(2) 
DIST   1.252,.01= C(1) TO O(1) 
DIST   1.252,.01= C(1) TO O(1,6,1,1,1) 
DIST   1.388,.01= C(2) TO C(3) 
DIST   1.388,.01= C(2) TO C(3,6,1,1,1) 
DIST   1.389,.01= C(3) TO C(4) 
DIST   1.392,.01= C(4) TO C(5) 
DIST   1.495,.01= C(4) TO C(6) 
DIST   1.248,.01= C(6) TO O(2) 
DIST   1.248,.01= C(6) TO O(3) 
DIST   1.420,.01= C(7) TO O(1) 
DIST   1.383,.01= C(8) TO O(4) 
ANGL 118,1= O(1) TO C(1) TO C(2) 
ANGL 118,1= O(1,6,1,1,1) TO C(1) TO C(2) 
ANGL 125,1= O(1,6,1,1,1) TO C(1) TO O(1) 
ANGL 120,1= C(3) TO C(2) TO C(1) 
ANGL 120,1= C(3,6,1,1,1) TO C(2) TO C(1) 
ANGL 120,1= C(3,6,1,1,1) TO C(2) TO C(3) 
ANGL 120,1= C(4) TO C(3) TO C(2) 
ANGL 120,1= C(5) TO C(4) TO C(3) 
ANGL 120,1= C(6) TO C(4) TO C(3) 
ANGL 120,1= C(6) TO C(4) TO C(5) 
ANGL 120,1= C(4,6,1,1,1) TO C(5) TO C(4) 
ANGL 117,1= O(2) TO C(6) TO C(4) 
ANGL 117,1= O(3) TO C(6) TO C(4) 
ANGL 125,1= O(3) TO C(6) TO O(2) 
ANGL 126,1= C(7) TO O(1) TO C(1) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = C(1) TO O(1,6,1,1,1) 
VIBR .0, 0.00200 = C(1) TO C(2) 
VIBR .0, 0.00200 = C(1) TO O(1) 
VIBR .0, 0.00500 = C(2) TO O(1,6,1,1,1) 
VIBR .0, 0.00500 = O(1) TO O(1,6,1,1,1) 
VIBR .0, 0.00500 = O(1) TO C(2) 
VIBR .0, 0.00200 = C(2) TO C(3,6,1,1,1) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00500 = C(3,6,1,1,1) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(3,6,1,1,1) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00200 = C(4) TO C(5) 
VIBR .0, 0.00200 = C(4) TO C(6) 
VIBR .0, 0.00500 = C(5) TO C(3) 
VIBR .0, 0.00500 = C(6) TO C(3) 
VIBR .0, 0.00500 = C(6) TO C(5) 
VIBR .0, 0.00500 = C(4) TO C(4,6,1,1,1) 
VIBR .0, 0.00200 = C(6) TO O(2) 
VIBR .0, 0.00200 = C(6) TO O(3) 
VIBR .0, 0.00500 = O(2) TO C(4) 
VIBR .0, 0.00500 = O(3) TO C(4) 
VIBR .0, 0.00500 = O(3) TO O(2) 
VIBR .0, 0.00200 = C(7) TO O(1) 
VIBR .0, 0.00200 = C(8) TO O(4) 
VIBR .0, 0.00500 = C(1) TO C(7) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = C(1) TO O(1,6,1,1,1) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.04000 = C(1) TO O(1) 
U(IJ) .0, 0.04000 = C(2) TO C(3,6,1,1,1) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(4) TO C(5) 
U(IJ) .0, 0.04000 = C(4) TO C(6) 
U(IJ) .0, 0.08000 = C(6) TO O(2) 
U(IJ) .0, 0.08000 = C(6) TO O(3) 
U(IJ) .0, 0.04000 = C(7) TO O(1) 
U(IJ) .0, 0.08000 = C(8) TO O(4) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
   0  13   4  x   .
  -1  15   3  x   .
  -2  17   0  x   .
  -1  13   0  x   .
  -8   8   4  x   .
  -1   8   6  x   .
  -1   1   1  x   .
  -1  14   2  x   .
  -3   4   5  x   .
 -12  18   1  x   .
 -11  11   5  x   .
  -2   4   1  x   .
  -2  15   1  x   .
  -3  17   1  x   .

#===END

data_st1006
_audit_creation_date        "12-10-02"
_audit_creation_method CRYSTALS_ver_14.40

 
_publ_contact_author_name         'Stephen A. Moggach' 
_publ_contact_author_address 
; 
 Dr Stephen Moggach 
 RSE Personal Research Fellow 
 The University of Edinburgh 
 Joseph Black Building 
 West Mains Road 
 Edinburgh 
 EH9 3JJ 
; 
 
_publ_contact_author_phone        '+44(0)131 6504806' 
_publ_contact_author_email        'smoggach@staffmail.ed.ac.uk' 
 
;
#===============================================================================

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

022_ALERT_3_B Ratio Unique / Expected Reflections (too) Low ..       0.74       
029_ALERT_3_B _diffrn_measured_fraction_theta_full Low .......       0.75 
341_ALERT_3_B Low Bond Precision on  C-C Bonds ...............      16.00 Ang. 
023_ALERT_3_C Resolution (too) Low [sin(theta)/Lambda < 0.6]..      15.75 Deg.
911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.559        285
913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....         11 
088_ALERT_3_G Poor Data / Parameter Ratio ....................       8.74  
 

The high pressure cell causes shading of a significant proportion of the
sphere of reflections. This means that the completeness is reduced and as
such the quality of the model is lower.All of the above are cause by shading 
by the pressure cell.

      
199_ALERT_1_B Check the Reported _cell_measurement_temperature        293 K     
200_ALERT_1_B Check the Reported   _diffrn_ambient_temperature        293 K  

correct

 
301_ALERT_3_B Note: Main Residue  Disorder ...................          5 %   

C7 is disordered 
  
 
601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of .        208 Ang3 
043_ALERT_1_C Check Reported Molecular Weight ................     971.23       
044_ALERT_1_C Calculated and Reported Dx Differ ..............          ?
041_ALERT_1_G Calc. and Reported SumFormula    Strings  Differ          ?
042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ          ?

Structure is a porous framework with disordered solvent in the pores.
The solvent region was treated by the van der Sluis and Spek method. 
See below. This corresponds to 1 molecule of IPA per formula unit. 
F(000), M, mu, D and the given formulae have been calculated on this 
assumption.

 
773_ALERT_2_B Check long C-C Bond in CIF: C7     --  C7      .       1.83 Ang. 
779_ALERT_4_B Suspect or Irrelevant (Bond) Angle in CIF .... #                
              H71  -C7   -C7     12.558   1.555  12.558                         
779_ALERT_4_B Suspect or Irrelevant (Bond) Angle in CIF .... #                
              H71  -C7   -H71    12.558   1.555   1.555                         
779_ALERT_4_B Suspect or Irrelevant (Bond) Angle in CIF .... #                
              C7   -C7   -H71    12.558   1.555   1.555  

not a real bond

                       
020_ALERT_3_G The value of Rint is greater than 0.12 .........       0.14 

This is becuase the data is weak


045_ALERT_1_G Calculated and Reported Z Differ by ............       3.00 Ratio 

due to choice of formula unit

     
220_ALERT_2_G Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       3.30 Ratio 
250_ALERT_2_G Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.35 

this is caused by C7 which is disordered and subject to thermal motion.
Half occupied carbon refined anistropically.


241_ALERT_2_G Check High      Ueq as Compared to Neighbors for         O2     
242_ALERT_2_G Check Low       Ueq as Compared to Neighbors for        Cu1

O2 next to heavy atom Cu1

     
      
731_ALERT_1_G Bond    Calc     1.25(2), Rep    1.252(7) ......          3 su-Rat
              O1   -C1      1.555   1.555                                       
731_ALERT_1_G Bond    Calc     1.48(2), Rep    1.476(8) ......          3 su-Rat
              C1   -C2      1.555   1.555                                       
731_ALERT_1_G Bond    Calc     1.40(2), Rep    1.401(6) ......          3 su-Rat
              C2   -C3      1.555   9.555                                       
731_ALERT_1_G Bond    Calc   1.400(13), Rep    1.401(6) ......          2 su-Rat
              C2   -C3      1.555   1.555                                       
731_ALERT_1_G Bond    Calc   1.387(17), Rep    1.387(6) ......          3 su-Rat
              C4   -C5      1.555   1.555                                       
732_ALERT_1_G Angle   Calc   117.6(11), Rep    117.6(3) ......       3.67 su-Rat
              O1   -C1   -C2      1.555   1.555   1.555                         
732_ALERT_1_G Angle   Calc   119.8(11), Rep    119.7(5) ......       2.20 su-Rat
              C2   -C3   -C4      1.555   1.555   1.555                         
732_ALERT_1_G Angle   Calc    120.4(9), Rep    120.3(4) ......       2.25 su-Rat
              C3   -C4   -C6      1.555   1.555   1.555                         
752_ALERT_4_G Angle   Calc      120.02, Rep    120.0(3) ......  Senseless su    
              C1   -C2   -C3      1.555   1.555   1.555

The use of restraints in the refinement mean that off diagonal terms in the
variance-covariance matrix are significant, and the diagonal approximation
used in Platon/Checkcif is badly in error.

                         
764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) .       1.13 Ratio 
      
no action taken
#===============================================================================
;
 
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000 -0.008       201        64 ' '
   2  0.333  0.667 -0.046       140        14 ' '
   3  0.667  0.333  0.000       140        14 ' '
_platon_squeeze_details
;
see above for details
;


_publ_section_exptl_refinement 
; 
; 
 
_publ_section_exptl_prep 
# Brief details or a reference. Include solvent if known 
; 
? 
; 
 
#end of refcif 
_cell_length_a                    18.577(2)
_cell_length_b                    18.577(2)
_cell_length_c                    6.8406(9)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      2044.4(4)
 
_symmetry_cell_setting            'trigonal' 
_symmetry_space_group_name_H-M    'P -3 m 1 ' 
_symmetry_space_group_name_Hall   '-P 3 2"' 
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 '-x,-y,-z'
 '-y,x-y,z'
 'y,-x+y,-z'
 '-x+y,-x,z'
 'x-y,x,-z'
 '-x+y,y,z'
 'x-y,-y,-z'
 'x,x-y,z'
 '-x,-x+y,-z'
 '-y,-x,z'
 'y,x,-z'

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source  
 C       0.0010   0.0010   2.3100  20.8439   1.0200  10.2075   1.5886   0.5687
   0.8650  51.6512   0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 H       0.0000   0.0000   0.4930  10.5109   0.3229  26.1257   0.1402   3.1424
   0.0408  57.7998   0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 O       0.0040   0.0030   3.0485  13.2771   2.2868   5.7011   1.5463   0.3239
   0.8670  32.9089   0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 Cu      0.2950   0.6370  13.3380   3.5828   7.1676   0.2470   5.6158  11.3966
   1.6735  64.8126   1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 
 
_cell_formula_units_Z                    2

# Given Formula = C30 H21 Cu3 O21 
# Dc =      1.48 Fooo =    918.00 Mu =     16.22 M =    151.35
# Found Formula = C30 H24 Cu3 O21 
# Dc =      1.48 FOOO =    918.00 Mu =     16.22 M =    151.86

_chemical_formula_sum             'C33 H32 Cu3 O22'
_chemical_formula_moiety          'C30 H24 Cu3 O21.(CH3)2CHOH'
_chemical_compound_source                ?
_chemical_formula_weight            971.23
 
 
_cell_measurement_reflns_used            1156
_cell_measurement_theta_min              2
_cell_measurement_theta_max              16
_cell_measurement_temperature          293
 
_exptl_crystal_description        'block' 
_exptl_crystal_colour             'crystal' 
_exptl_crystal_size_min           0.100 
_exptl_crystal_size_mid           0.200 
_exptl_crystal_size_max           0.200 
 
_exptl_crystal_density_diffrn     1.578 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              986 
_exptl_absorpt_coefficient_mu     0.534
 
# Sheldrick geometric approximatio 0.72 0.85 
# No experimental values of Tmin/max available 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'SADABS (Siemens, 1996)' 
_exptl_absorpt_correction_T_min   0.72 
_exptl_absorpt_correction_T_max   0.85 
_diffrn_measurement_device_type   'Rigaku Saturn 724+' 
_diffrn_measurement_device        'Area' 
_diffrn_radiation_monochromator   'graphite' 
_diffrn_radiation_type            'synchrotron'
_diffrn_radiation_wavelength           0.48590
_diffrn_measurement_method        ω 
 
# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection        'USER DEFINED DATA COLLECTION' 
_computing_cell_refinement        'USER DEFINED CELL REFINEMENT' 
_computing_data_reduction         'USER DEFINED DATA REDUCTION' 
_computing_structure_solution     'USER DEFINED STRUCTURE SOLUTION' 
_computing_structure_refinement   'CRYSTALS (Betteridge et al., 2003)' 
_computing_publication_material   'CRYSTALS (Betteridge et al., 2003)' 
_computing_molecular_graphics     'CAMERON (Watkin et al., 1996)' 
 
_diffrn_standards_interval_time   . 
_diffrn_standards_interval_count  . 
_diffrn_standards_number          0 
_diffrn_standards_decay_%         ? 
 
_diffrn_ambient_temperature        293
_diffrn_reflns_number             4771 
_reflns_number_total              830 
_diffrn_reflns_av_R_equivalents   0.1356 
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 831 
# Theoretical number of reflections is about 1991 
 
 
_diffrn_reflns_theta_min          0.865 
_diffrn_reflns_theta_max          15.751 
_diffrn_measured_fraction_theta_max 0.743 
 
_diffrn_reflns_theta_full         15.436 
_diffrn_measured_fraction_theta_full 0.745 
 
 
_diffrn_reflns_limit_h_min        -17 
_diffrn_reflns_limit_h_max        0 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        20 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        7 
_reflns_limit_h_min               -17 
_reflns_limit_h_max               0 
_reflns_limit_k_min               0 
_reflns_limit_k_max               20 
_reflns_limit_l_min               0 
_reflns_limit_l_max               7 
 
_oxford_diffrn_Wilson_B_factor    0.00 
_oxford_diffrn_Wilson_scale       0.00 
 
_atom_sites_solution_primary      Other  #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    difmap
 
_refine_diff_density_min          -0.74 
_refine_diff_density_max          0.76 
 
 
# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 
 
 
# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref     I>-10.0\s(I)
_refine_ls_number_reflns          822 
_refine_ls_number_restraints      116 
_refine_ls_number_parameters      94 
_oxford_refine_ls_R_factor_ref    0.1221 
_refine_ls_wR_factor_ref          0.2159 
_refine_ls_goodness_of_fit_ref    0.9858 
_refine_ls_shift/su_max           0.0004119 
_refine_ls_shift/su_mean          0.0000092 
 
 
# The values computed with all filters except I/sigma 
_oxford_reflns_number_all         822 
_refine_ls_R_factor_all           0.1221 
_refine_ls_wR_factor_all          0.2159 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0σ(I)
_reflns_number_gt                 470 
_refine_ls_R_factor_gt            0.0678 
_refine_ls_wR_factor_gt           0.1562 
 
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration  '.' 
 
 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full
_refine_ls_hydrogen_treatment     noref          #undef, noref, refall,
                                                 # refxyz, refU, constr or mixed
 
# WARNING. The IUCr will not accept Unit Weights 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
;
 Method= Quasi-Unit weights 
 W = 1.0 or 1./2F 
;
# Insert your own references if required - in alphabetical order 
_publ_section_references 
; 
User-defined structure solution reference 
 
User-defined data collection reference 
 
User defined data reduction 
 
User defined cell refinement 
 
Betteridge, P.W., Carruthers, J.R., Cooper, R.I., 
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 
 
Siemens Industrial Automation, Inc (1996). 
SADABS: Area-Detector Absorption Correction;: Madison, WI. 
 
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical 
Crystallography Laboratory, Oxford, UK. 
; 

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cu1 Cu 0.52351(6) 0.47649(6) 0.3438(3) 0.0294 1.0000 Uani S T . . . . 
O1 O 0.2840(9) 0.2017(6) 1.2531(16) 0.1046 1.0000 Uani D U . . . . 
O2 O 0.4801(6) 0.3708(5) 0.4832(10) 0.0507 1.0000 Uani D U . . . . 
O3 O 0.4401(6) 0.4101(5) 0.7498(10) 0.0507 1.0000 Uani D U . . . . 
O4 O 0.5624(4) 0.4376(4) 0.0877(16) 0.0546 1.0000 Uani S T . . . . 
H42 H 0.5243 0.4176 0.0130 0.0600 1.0000 Uiso . . . . . . 
C1 C 0.3036(14) 0.1518(7) 1.182(2) 0.0703 1.0000 Uani DS TU . . . . 
C2 C 0.3542(11) 0.1771(5) 1.0019(18) 0.0470 1.0000 Uani DS TU . . . . 
C3 C 0.3775(8) 0.2540(5) 0.9154(13) 0.0491 1.0000 Uani D U . . . . 
C4 C 0.4224(7) 0.2761(4) 0.7433(11) 0.0378 1.0000 Uani D U . . . . 
C5 C 0.4403(10) 0.2202(5) 0.6521(16) 0.0375 1.0000 Uani DS TU . . . . 
C6 C 0.4486(7) 0.3584(4) 0.6501(10) 0.0334 1.0000 Uani D U . . . . 
C7 C 0.232(2) 0.1864(16) 1.420(4) 0.1106 0.5000 Uani D U . . . . 
H31 H 0.3675 0.2921 0.9788 0.0600 1.0000 Uiso . . . . . . 
H51 H 0.4740 0.2370 0.5324 0.0600 1.0000 Uiso . . . . . . 
H71 H 0.2296 0.2348 1.4452 0.1264 0.5000 Uiso . . . . . . 
H72 H 0.2650 0.1790 1.5331 0.1264 0.5000 Uiso . . . . . . 
H73 H 0.1818 0.1371 1.4057 0.1264 0.5000 Uiso . . . . . . 
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0305(9) 0.0305(9) 0.0327(10) 0.0009(4) -0.0009(4) 0.0192(9) 
O1 0.138(11) 0.093(8) 0.113(8) 0.017(7) 0.069(7) 0.081(8) 
O2 0.077(7) 0.044(5) 0.046(4) 0.006(3) 0.023(4) 0.040(5) 
O3 0.080(7) 0.040(4) 0.044(4) 0.007(4) 0.020(4) 0.040(5) 
O4 0.059(6) 0.059(6) 0.041(6) 0.003(3) -0.003(3) 0.025(7) 
C1 0.098(14) 0.055(5) 0.072(11) 0.023(5) 0.045(9) 0.049(7) 
C2 0.057(10) 0.042(4) 0.047(8) 0.006(3) 0.013(6) 0.029(5) 
C3 0.067(8) 0.050(6) 0.044(6) 0.010(4) 0.013(5) 0.040(6) 
C4 0.045(6) 0.030(4) 0.038(5) -0.005(3) 0.000(4) 0.018(5) 
C5 0.045(10) 0.033(4) 0.039(8) 0.002(3) 0.004(6) 0.023(5) 
C6 0.036(6) 0.037(4) 0.035(4) 0.000(3) 0.003(4) 0.024(5) 
C7 0.13(2) 0.120(19) 0.083(17) -0.023(11) 0.043(11) 0.066(18) 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 0.2659(10) 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
Cu1 . O3 12_556 1.970(7)    yes
Cu1 . O3 2_666 1.970(7)    yes
Cu1 . O2 11_665 1.957(7)    yes
Cu1 . Cu1 2_666 2.618(4)    yes
Cu1 . O2 . 1.957(7)    yes
Cu1 . O4 . 2.154(12)    yes
O1 . C1 . 1.252(7)    yes
O1 . C7 . 1.431(9)    yes
O2 . C6 . 1.251(7)    yes
O3 . C6 . 1.250(7)    yes
O4 . H42 11_665 0.798    no
O4 . H42 . 0.798    no
C1 . C2 . 1.476(8)    yes
C2 . C3 9_555 1.401(6)    yes
C2 . C3 . 1.401(6)    yes
C3 . C4 . 1.381(7)    yes
C3 . H31 . 0.924    no
C4 . C5 . 1.387(6)    yes
C4 . C6 . 1.496(7)    yes
C5 . H51 . 0.981    no
C7 . H71 12_558 1.206    no
C7 . C7 12_558 1.83(3)    yes
C7 . H71 . 0.936    no
C7 . H72 . 1.039    no
C7 . H73 . 0.928    no
H71 . H71 12_558 0.767    no
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
O3 12_556 Cu1 . O3 2_666 89.8(5)    yes
O3 12_556 Cu1 . O2 11_665 168.5(3)    yes
O3 2_666 Cu1 . O2 11_665 88.9(4)    yes
O3 12_556 Cu1 . Cu1 2_666 84.4(2)    yes
O3 2_666 Cu1 . Cu1 2_666 84.4(2)    yes
O2 11_665 Cu1 . Cu1 2_666 84.2(2)    yes
O3 12_556 Cu1 . O2 . 88.9(4)    yes
O3 2_666 Cu1 . O2 . 168.5(3)    yes
O2 11_665 Cu1 . O2 . 90.1(5)    yes
Cu1 2_666 Cu1 . O2 . 84.18(19)    yes
O3 12_556 Cu1 . O4 . 95.8(3)    yes
O3 2_666 Cu1 . O4 . 95.8(3)    yes
O2 11_665 Cu1 . O4 . 95.7(3)    yes
Cu1 2_666 Cu1 . O4 . 179.8(4)    yes
O2 . Cu1 . O4 . 95.7(3)    yes
C1 . O1 . C7 . 125.6(8)    yes
Cu1 . O2 . C6 . 123.3(5)    yes
Cu1 2_666 O3 . C6 . 122.4(5)    yes
Cu1 . O4 . H42 11_665 108.0    no
Cu1 . O4 . H42 . 108.0    no
H42 11_665 O4 . H42 . 85.1    no
O1 . C1 . O1 9_555 124.7(7)    yes
O1 . C1 . C2 . 117.6(3)    yes
O1 9_555 C1 . C2 . 117.6(3)    yes
C1 . C2 . C3 9_555 120.0(3)    yes
C1 . C2 . C3 . 120.0(3)    yes
C3 9_555 C2 . C3 . 119.9(6)    yes
C2 . C3 . C4 . 119.7(5)    yes
C2 . C3 . H31 . 120.3    no
C4 . C3 . H31 . 119.8    no
C3 . C4 . C5 . 119.8(5)    yes
C3 . C4 . C6 . 120.3(4)    yes
C5 . C4 . C6 . 119.8(4)    yes
C4 . C5 . C4 9_555 120.6(6)    yes
C4 . C5 . H51 . 119.3    no
C4 9_555 C5 . H51 . 119.3    no
C4 . C6 . O2 . 117.4(5)    yes
C4 . C6 . O3 . 116.8(5)    yes
O2 . C6 . O3 . 125.7(5)    yes
O1 . C7 . H71 12_558 132.6    no
O1 . C7 . C7 12_558 144.0(19)    yes
H71 12_558 C7 . C7 12_558 27.3    no
O1 . C7 . H71 . 107.8    no
H71 12_558 C7 . H71 . 39.5    no
C7 12_558 C7 . H71 . 36.2    no
O1 . C7 . H72 . 103.5    no
H71 12_558 C7 . H72 . 71.8    no
C7 12_558 C7 . H72 . 93.2    no
H71 . C7 . H72 . 107.6    no
O1 . C7 . H73 . 110.8    no
H71 12_558 C7 . H73 . 115.3    no
C7 12_558 C7 . H73 . 93.1    no
H71 . C7 . H73 . 117.6    no
H72 . C7 . H73 . 108.4    no
C7 12_558 H71 . H71 12_558 50.9    no
C7 12_558 H71 . C7 . 116.5    no
H71 12_558 H71 . C7 . 89.6    no


_iucr_refine_instruction_details_constraints
;
#
# Punched on 02/10/12 at 14:43:20
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
END                                                                             
;


_iucr_refine_instruction_details_restraints
;
#
# Punched on 02/10/12 at 14:43:20
#
#LIST     16                                                                    
DIST   1.252,.01= O(1) TO C(1) 
DIST   1.427,.01= O(1) TO C(7) 
DIST   1.245,.01= O(2) TO C(6) 
DIST   1.254,.01= O(3) TO C(6) 
DIST   1.476,.01= C(1) TO C(2) 
DIST   1.396,.01= C(2) TO C(3) 
DIST   1.396,.01= C(2) TO C(3,5) 
DIST   1.376,.01= C(3) TO C(4) 
DIST   1.391,.01= C(4) TO C(5) 
DIST   1.497,.01= C(4) TO C(6) 
ANGL 125,1= C(7) TO O(1) TO C(1) 
ANGL 125,1= O(1,5) TO C(1) TO O(1) 
ANGL 118,1= C(2) TO C(1) TO O(1) 
ANGL 118,1= C(2) TO C(1) TO O(1,5) 
ANGL 120,1= C(3) TO C(2) TO C(1) 
ANGL 120,1= C(3,5) TO C(2) TO C(1) 
ANGL 120,1= C(3,5) TO C(2) TO C(3) 
ANGL 120,1= C(4) TO C(3) TO C(2) 
ANGL 120,1= C(5) TO C(4) TO C(3) 
ANGL 120,1= C(6) TO C(4) TO C(3) 
ANGL 120,1= C(6) TO C(4) TO C(5) 
ANGL 121,1= C(4,5) TO C(5) TO C(4) 
ANGL 125,1= O(3) TO C(6) TO O(2) 
ANGL 117,1= C(4) TO C(6) TO O(2) 
ANGL 117,1= C(4) TO C(6) TO O(3) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = O(1) TO C(1) 
VIBR .0, 0.00200 = O(1) TO C(7) 
VIBR .0, 0.00500 = C(7) TO C(1) 
VIBR .0, 0.00200 = O(2) TO C(6) 
VIBR .0, 0.00200 = O(3) TO C(6) 
VIBR .0, 0.00200 = C(1) TO C(2) 
VIBR .0, 0.00500 = O(1) TO O(1,5) 
VIBR .0, 0.00500 = C(2) TO O(1,5) 
VIBR .0, 0.00500 = C(2) TO O(1) 
VIBR .0, 0.00200 = C(2) TO C(3,5) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00500 = C(3,5) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(3,5) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00200 = C(4) TO C(5) 
VIBR .0, 0.00200 = C(4) TO C(6) 
VIBR .0, 0.00500 = C(5) TO C(3) 
VIBR .0, 0.00500 = C(6) TO C(3) 
VIBR .0, 0.00500 = C(6) TO C(5) 
VIBR .0, 0.00500 = C(4) TO C(4,5) 
VIBR .0, 0.00500 = O(2) TO C(4) 
VIBR .0, 0.00500 = O(3) TO C(4) 
VIBR .0, 0.00500 = O(3) TO O(2) 
VIBR .0, 0.00200 = C(7) TO C(7,-6,1,0,0,3) 
VIBR .0, 0.00500 = C(7,-6,1,0,0,3) TO O(1) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = O(1) TO C(1) 
U(IJ) .0, 0.04000 = O(1) TO C(7) 
U(IJ) .0, 0.08000 = O(2) TO C(6) 
U(IJ) .0, 0.08000 = O(3) TO C(6) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.04000 = C(2) TO C(3,5) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(4) TO C(5) 
U(IJ) .0, 0.04000 = C(4) TO C(6) 
U(IJ) .0, 0.04000 = C(7) TO C(7,-6,1,0,0,3) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
  -4  18   3  x   .
 -10  17   4  x   .
  -8  12   6  x   .
  -6  15   5  x   .
  -8  16   2  x   .
  -9  20   1  x   .
  -4  12   6  x   .
   0   1   0  x   .

#===END

data_st1007
_audit_creation_date        "12-10-02"
_audit_creation_method CRYSTALS_ver_14.40

_oxford_structure_analysis_title  'stam15 in P-3m1'
_chemical_name_systematic         ?
_chemical_melting_point           ?


_publ_contact_author_name         'Stephen A. Moggach' 
_publ_contact_author_address 
;

 Dr Stephen Moggach 
 RSE Personal Research Fellow 
 The University of Edinburgh 
 Joseph Black Building 
 West Mains Road 
 Edinburgh 
 EH9 3JJ 
; 
 
_publ_contact_author_phone        '+44(0)131 6504806' 
_publ_contact_author_email        'smoggach@staffmail.ed.ac.uk' 

;
#===============================================================================

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

       
043_ALERT_1_B Check Reported Molecular Weight ................    1031.33       
044_ALERT_1_B Calculated and Reported Dx Differ ..............          ?
041_ALERT_1_G Calc. and Reported SumFormula    Strings  Differ          ?
042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ          ?
601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of .        197 Ang3 

Structure is a porous framework with disordered solvent in the pores.
The solvent region was treated by the van der Sluis and Spek method. 
See below. This corresponds to 2 molecules of IPA per formula unit. 
F(000), M, mu, D and the given formulae have been calculated on this 
assumption.


029_ALERT_3_B _diffrn_measured_fraction_theta_full Low .......       0.74
341_ALERT_3_B Low Bond Precision on  C-C Bonds ...............      17.00 Ang.
088_ALERT_3_G Poor Data / Parameter Ratio ....................       8.36
084_ALERT_3_G High wR2 Value (i.e. > 0.25) ...................       0.26 

The high pressure cell causes shading of a significant proportion of the
sphere of reflections. This means that the completeness is reduced and as
such the quality of the model is lower.All of the above are cause by shading 
by the pressure cell. 

199_ALERT_1_B Check the Reported _cell_measurement_temperature        293 K     
200_ALERT_1_B Check the Reported   _diffrn_ambient_temperature        293 K

correct

     
301_ALERT_3_B Note: Main Residue  Disorder ...................          5 % 
250_ALERT_2_G Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.53 
220_ALERT_2_G Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       3.39 Ratio 

this is caused by C7 which is disordered and subject to thermal motion.
Half occupied carbon refined anistropically. 
    
  
411_ALERT_2_B Short Inter H...H Contact  H71    ..  H72     ..       1.39 Ang.  
411_ALERT_2_B Short Inter H...H Contact  H71    ..  H73     ..       1.62 Ang.  
779_ALERT_4_B Suspect or Irrelevant (Bond) Angle in CIF .... #                
              C7   -C7   -H71    12.558   1.555   1.555       

NOt real bonds

045_ALERT_1_G Calculated and Reported Z Differ by ............       3.00 Ratio 

due to choice of forumla unit


731_ALERT_1_C Bond    Calc     1.24(3), Rep    1.243(7) ......          4 su-Rat
              O1   -C1      1.555   1.555                                       
732_ALERT_1_C Angle   Calc   118.0(13), Rep    118.0(3) ......       4.33 su-Rat
              O1   -C1   -C2      1.555   1.555   1.555                         
732_ALERT_1_C Angle   Calc   120.1(15), Rep    120.0(3) ......       5.00 su-Rat
              C1   -C2   -C3      1.555   1.555   1.555 
731_ALERT_1_G Bond    Calc     1.48(2), Rep    1.484(8) ......          3 su-Rat
              C1   -C2      1.555   1.555                                       
731_ALERT_1_G Bond    Calc     1.40(2), Rep    1.403(6) ......          3 su-Rat
              C2   -C3      1.555   9.555                                       
731_ALERT_1_G Bond    Calc   1.402(14), Rep    1.403(6) ......          2 su-Rat
              C2   -C3      1.555   1.555                                       
731_ALERT_1_G Bond    Calc   1.382(15), Rep    1.382(7) ......          2 su-Rat
              C3   -C4      1.555   1.555                                       
731_ALERT_1_G Bond    Calc   1.384(19), Rep    1.385(7) ......          3 su-Rat
              C4   -C5      1.555   1.555                                       
732_ALERT_1_G Angle   Calc   119.6(12), Rep    119.6(5) ......       2.40 su-Rat
              C2   -C3   -C4      1.555   1.555   1.555                         
732_ALERT_1_G Angle   Calc   120.4(10), Rep    120.4(4) ......       2.50 su-Rat
              C3   -C4   -C6      1.555   1.555   1.555                         
732_ALERT_1_G Angle   Calc    119.8(9), Rep    119.8(4) ......       2.25 su-Rat
              C5   -C4   -C6      1.555   1.555   1.555 


The use of restraints in the refinement mean that off diagonal terms in the
variance-covariance matrix are significant, and the diagonal approximation
used in Platon/Checkcif is badly in error.  
      

241_ALERT_2_G Check High      Ueq as Compared to Neighbors for         O1     
241_ALERT_2_G Check High      Ueq as Compared to Neighbors for         O2     
242_ALERT_2_G Check Low       Ueq as Compared to Neighbors for        Cu1 

Cu1 is a heavy atom
   
      
                        
764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) .       1.13 Ratio

no action taken 

#===============================================================================
;


loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000 -0.008       176        94 ' '
   2  0.333  0.667 -0.051       133        42 ' '
   3  0.667  0.333  0.005       133        42 ' '
_platon_squeeze_details
;
see above for details
; 
 
_publ_section_exptl_refinement 
; 
; 
 
_publ_section_exptl_prep 
# Brief details or a reference. Include solvent if known 
; 
? 
; 
 
#end of refcif 
_cell_length_a                    18.459(2)
_cell_length_b                    18.459(2)
_cell_length_c                    6.7489(9)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      1991.6(4)
 
_symmetry_cell_setting            'trigonal' 
_symmetry_space_group_name_H-M    'P -3 m 1 ' 
_symmetry_space_group_name_Hall   '-P 3 2"' 
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 '-x,-y,-z'
 '-y,x-y,z'
 'y,-x+y,-z'
 '-x+y,-x,z'
 'x-y,x,-z'
 '-x+y,y,z'
 'x-y,-y,-z'
 'x,x-y,z'
 '-x,-x+y,-z'
 '-y,-x,z'
 'y,x,-z'

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source  
 C       0.0033   0.0016   2.3100  20.8439   1.0200  10.2075   1.5886   0.5687
   0.8650  51.6512   0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 H       0.0000   0.0000   0.4930  10.5109   0.3229  26.1257   0.1402   3.1424
   0.0408  57.7998   0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 O       0.0106   0.0060   3.0485  13.2771   2.2868   5.7011   1.5463   0.3239
   0.8670  32.9089   0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 Cu      0.3201   1.2651  13.3380   3.5828   7.1676   0.2470   5.6158  11.3966
   1.6735  64.8126   1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 
 
_cell_formula_units_Z                    2

# Given Formula = C30 H21 Cu3 O21 
# Dc =      1.51 Fooo =    915.00 Mu =     16.65 M =    151.35
# Found Formula = C30 H22.50 Cu3 O21 
# Dc =      1.52 FOOO =    915.00 Mu =     16.65 M =    151.61

_chemical_formula_sum             'C36 H40 Cu3 O23'
_chemical_formula_moiety          'C30 H24 Cu3 O21.2(CH3)2CHOH'
_chemical_compound_source                ?
_chemical_formula_weight            1031.33
 
 
_cell_measurement_reflns_used         1087
_cell_measurement_theta_min              2
_cell_measurement_theta_max             16
_cell_measurement_temperature          293
 
_exptl_crystal_description        'block' 
_exptl_crystal_colour             'crystal' 
_exptl_crystal_size_min           0.100 
_exptl_crystal_size_mid           0.200 
_exptl_crystal_size_max           0.200 
 
_exptl_crystal_density_diffrn     1.720 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              1054 
_exptl_absorpt_coefficient_mu     0.549 
 
# Sheldrick geometric approximatio 1.00 1.00 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'SADABS (Siemens, 1996)' 
_exptl_absorpt_correction_T_min   0.58
_exptl_absorpt_correction_T_max   0.74 
_diffrn_measurement_device_type   'Rigaku Saturn 724+' 
_diffrn_measurement_device        'Area' 
_diffrn_radiation_monochromator   'graphite' 
_diffrn_radiation_type            'synchrotron'
_diffrn_radiation_wavelength           0.48590
_diffrn_measurement_method        ω 

 
# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection        'USER DEFINED DATA COLLECTION' 
_computing_cell_refinement        'USER DEFINED CELL REFINEMENT' 
_computing_data_reduction         'USER DEFINED DATA REDUCTION' 
_computing_structure_solution     'USER DEFINED STRUCTURE SOLUTION' 
_computing_structure_refinement   'CRYSTALS (Betteridge et al., 2003)' 
_computing_publication_material   'CRYSTALS (Betteridge et al., 2003)' 
_computing_molecular_graphics     'CAMERON (Watkin et al., 1996)' 
 
_diffrn_standards_interval_time   . 
_diffrn_standards_interval_count  . 
_diffrn_standards_number          0 
_diffrn_standards_decay_%         ? 
 
_diffrn_ambient_temperature        293
_diffrn_reflns_number             4707 
_reflns_number_total              799 
_diffrn_reflns_av_R_equivalents   0.1660 
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 799 
# Theoretical number of reflections is about 1929 
 
 
_diffrn_reflns_theta_min          1.274 
_diffrn_reflns_theta_max          23.351 
_diffrn_measured_fraction_theta_max 0.739 
 
_diffrn_reflns_theta_full         23.351 
_diffrn_measured_fraction_theta_full 0.739 
 
 
_diffrn_reflns_limit_h_min        -17 
_diffrn_reflns_limit_h_max        0 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        20 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        7 
_reflns_limit_h_min               -17 
_reflns_limit_h_max               0 
_reflns_limit_k_min               0 
_reflns_limit_k_max               20 
_reflns_limit_l_min               0 
_reflns_limit_l_max               7 
 
_oxford_diffrn_Wilson_B_factor    0.00 
_oxford_diffrn_Wilson_scale       0.00 
 
_atom_sites_solution_primary      Other  #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    difmap
 
_refine_diff_density_min          -1.12 
_refine_diff_density_max          1.34 
 
 
# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 
 
 
# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref     I>-10.0\s(I)
_refine_ls_number_reflns          786 
_refine_ls_number_restraints      116 
_refine_ls_number_parameters      94 
_oxford_refine_ls_R_factor_ref    0.1441 
_refine_ls_wR_factor_ref          0.2566 
_refine_ls_goodness_of_fit_ref    1.0066 
_refine_ls_shift/su_max           0.0002748 
_refine_ls_shift/su_mean          0.0000379 
 
 
# The values computed with all filters except I/sigma 
_oxford_reflns_number_all         786 
_refine_ls_R_factor_all           0.1441 
_refine_ls_wR_factor_all          0.2566 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0σ(I)
_reflns_number_gt                 410 
_refine_ls_R_factor_gt            0.0819 
_refine_ls_wR_factor_gt           0.2222 
 
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration  '.' 
 
 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full
_refine_ls_hydrogen_treatment     noref          #undef, noref, refall,
                                                 # refxyz, refU, constr or mixed
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.13P)² +15.34P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
# Insert your own references if required - in alphabetical order 
_publ_section_references 
; 
User-defined structure solution reference 
 
User-defined data collection reference 
 
User defined data reduction 
 
User defined cell refinement 
 
Betteridge, P.W., Carruthers, J.R., Cooper, R.I., 
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 
 
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical 
Crystallography Laboratory, Oxford, UK. 
; 

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cu1 Cu 0.52401(6) 0.47599(6) 0.3425(3) 0.0350 1.0000 Uani S T . . . . 
O1 O 0.2869(10) 0.2029(6) 1.2728(18) 0.1312 1.0000 Uani D U . . . . 
O2 O 0.4800(7) 0.3717(6) 0.4844(12) 0.0693 1.0000 Uani D U . . . . 
O3 O 0.4409(6) 0.4114(5) 0.7546(12) 0.0572 1.0000 Uani D U . . . . 
O4 O 0.5637(4) 0.4363(4) 0.0795(19) 0.0602 1.0000 Uani S T . . . . 
H42 H 0.5242 0.4177 0.0095 0.0600 1.0000 Uiso . . . . . . 
C1 C 0.3068(16) 0.1534(8) 1.200(2) 0.0766 1.0000 Uani DS TU . . . . 
C2 C 0.3553(12) 0.1776(6) 1.0129(19) 0.0507 1.0000 Uani DS TU . . . . 
C3 C 0.3784(8) 0.2550(5) 0.9244(14) 0.0477 1.0000 Uani D U . . . . 
C4 C 0.4223(7) 0.2764(5) 0.7480(13) 0.0432 1.0000 Uani D U . . . . 
C5 C 0.4401(11) 0.2201(6) 0.6560(17) 0.0411 1.0000 Uani DS TU . . . . 
C6 C 0.4493(8) 0.3594(5) 0.6540(12) 0.0427 1.0000 Uani D U . . . . 
C7 C 0.232(2) 0.1858(17) 1.438(5) 0.1389 0.5000 Uani D U . . . . 
H31 H 0.3632 0.2920 0.9843 0.0567 1.0000 Uiso . . . . . . 
H71 H 0.2297 0.2297 1.5000 0.1656 1.0000 Uiso . . . . . . 
H72 H 0.2543 0.1722 1.5536 0.1656 0.5000 Uiso . . . . . . 
H73 H 0.1763 0.1371 1.4054 0.1656 0.5000 Uiso . . . . . . 
H51 H 0.4651 0.2326 0.5284 0.0487 1.0000 Uiso . . . . . . 
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0378(12) 0.0378(12) 0.0397(13) -0.0004(5) 0.0004(5) 0.0267(12) 
O1 0.184(13) 0.117(10) 0.124(10) 0.014(8) 0.087(9) 0.099(10) 
O2 0.126(10) 0.062(6) 0.053(5) 0.022(4) 0.031(5) 0.072(7) 
O3 0.068(7) 0.042(5) 0.066(5) -0.004(4) 0.013(5) 0.030(5) 
O4 0.062(7) 0.062(7) 0.061(9) 0.002(4) -0.002(4) 0.034(8) 
C1 0.105(15) 0.070(6) 0.067(11) 0.023(5) 0.046(10) 0.053(8) 
C2 0.058(11) 0.048(5) 0.049(8) 0.008(4) 0.016(7) 0.029(6) 
C3 0.058(9) 0.049(7) 0.044(6) 0.005(4) 0.012(5) 0.033(7) 
C4 0.046(7) 0.044(6) 0.049(6) 0.007(4) 0.013(5) 0.029(6) 
C5 0.051(11) 0.038(4) 0.039(9) 0.003(4) 0.007(7) 0.025(6) 
C6 0.052(8) 0.044(5) 0.044(5) 0.003(4) 0.005(5) 0.033(6) 
C7 0.16(2) 0.14(2) 0.11(2) -0.031(14) 0.066(14) 0.07(2) 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 0.917(16) 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
Cu1 . O3 2_666 1.956(8)    yes
Cu1 . O3 12_556 1.956(8)    yes
Cu1 . O2 11_665 1.928(8)    yes
Cu1 . Cu1 2_666 2.622(4)    yes
Cu1 . O2 . 1.928(8)    yes
Cu1 . O4 . 2.181(13)    yes
O1 . C1 . 1.243(7)    yes
O1 . C7 . 1.431(9)    yes
O2 . C6 . 1.248(7)    yes
O3 . C6 . 1.246(7)    yes
O4 . H42 11_665 0.789    no
O4 . H42 . 0.789    no
C1 . C2 . 1.484(8)    yes
C2 . C3 9_555 1.403(6)    yes
C2 . C3 . 1.403(6)    yes
C3 . C4 . 1.382(7)    yes
C3 . H31 . 0.950    no
C4 . C5 . 1.385(7)    yes
C4 . C6 . 1.495(7)    yes
C5 . H51 . 0.950    no
C7 . C7 12_558 1.70(4)    yes
C7 . H71 . 0.932    no
C7 . H72 . 0.971    no
C7 . H73 . 0.996    no
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
O3 2_666 Cu1 . O3 12_556 88.4(6)    yes
O3 2_666 Cu1 . O2 11_665 89.3(4)    yes
O3 12_556 Cu1 . O2 11_665 167.9(3)    yes
O3 2_666 Cu1 . Cu1 2_666 84.3(2)    yes
O3 12_556 Cu1 . Cu1 2_666 84.3(2)    yes
O2 11_665 Cu1 . Cu1 2_666 83.7(2)    yes
O3 2_666 Cu1 . O2 . 167.9(3)    yes
O3 12_556 Cu1 . O2 . 89.3(4)    yes
O2 11_665 Cu1 . O2 . 90.4(7)    yes
Cu1 2_666 Cu1 . O2 . 83.7(2)    yes
O3 2_666 Cu1 . O4 . 95.5(3)    yes
O3 12_556 Cu1 . O4 . 95.5(3)    yes
O2 11_665 Cu1 . O4 . 96.5(3)    yes
Cu1 2_666 Cu1 . O4 . 179.7(4)    yes
O2 . Cu1 . O4 . 96.5(3)    yes
C1 . O1 . C7 . 125.5(8)    yes
Cu1 . O2 . C6 . 124.3(5)    yes
Cu1 2_666 O3 . C6 . 122.2(5)    yes
Cu1 . O4 . H42 11_665 104.0    no
Cu1 . O4 . H42 . 104.0    no
H42 11_665 O4 . H42 . 85.6    no
O1 9_555 C1 . O1 . 124.0(7)    yes
O1 9_555 C1 . C2 . 118.0(3)    yes
O1 . C1 . C2 . 118.0(3)    yes
C1 . C2 . C3 9_555 120.0(3)    yes
C1 . C2 . C3 . 120.0(3)    yes
C3 9_555 C2 . C3 . 119.9(6)    yes
C2 . C3 . C4 . 119.6(5)    yes
C2 . C3 . H31 . 120.1    no
C4 . C3 . H31 . 120.2    no
C3 . C4 . C5 . 119.8(5)    yes
C3 . C4 . C6 . 120.4(4)    yes
C5 . C4 . C6 . 119.8(4)    yes
C4 9_555 C5 . C4 . 120.9(6)    yes
C4 9_555 C5 . H51 . 119.5    no
C4 . C5 . H51 . 119.5    no
C4 . C6 . O2 . 117.6(5)    yes
C4 . C6 . O3 . 116.9(5)    yes
O2 . C6 . O3 . 125.5(6)    yes
O1 . C7 . C7 12_558 139(3)    yes
O1 . C7 . H71 . 119.5    no
C7 12_558 C7 . H71 . 24.3    no
O1 . C7 . H72 . 109.8    no
C7 12_558 C7 . H72 . 96.8    no
H71 . C7 . H72 . 94.2    no
O1 . C7 . H73 . 109.0    no
C7 12_558 C7 . H73 . 90.6    no
H71 . C7 . H73 . 114.1    no
H72 . C7 . H73 . 108.9    no
C7 . H71 . C7 12_558 131.4    no


_iucr_refine_instruction_details_constraints
;
#
# Punched on 02/10/12 at 14:57:59
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
END                                                                             
;


_iucr_refine_instruction_details_restraints
;
#
# Punched on 02/10/12 at 14:57:59
#
#LIST     16                                                                    
DIST   1.252,.01= O(1) TO C(1) 
DIST   1.427,.01= O(1) TO C(7) 
DIST   1.245,.01= O(2) TO C(6) 
DIST   1.254,.01= O(3) TO C(6) 
DIST   1.476,.01= C(1) TO C(2) 
DIST   1.396,.01= C(2) TO C(3) 
DIST   1.396,.01= C(2) TO C(3,5) 
DIST   1.376,.01= C(3) TO C(4) 
DIST   1.391,.01= C(4) TO C(5) 
DIST   1.497,.01= C(4) TO C(6) 
ANGL 125,1= C(7) TO O(1) TO C(1) 
ANGL 125,1= O(1,5) TO C(1) TO O(1) 
ANGL 118,1= C(2) TO C(1) TO O(1) 
ANGL 118,1= C(2) TO C(1) TO O(1,5) 
ANGL 120,1= C(3) TO C(2) TO C(1) 
ANGL 120,1= C(3,5) TO C(2) TO C(1) 
ANGL 120,1= C(3,5) TO C(2) TO C(3) 
ANGL 120,1= C(4) TO C(3) TO C(2) 
ANGL 120,1= C(5) TO C(4) TO C(3) 
ANGL 120,1= C(6) TO C(4) TO C(3) 
ANGL 120,1= C(6) TO C(4) TO C(5) 
ANGL 121,1= C(4,5) TO C(5) TO C(4) 
ANGL 125,1= O(3) TO C(6) TO O(2) 
ANGL 117,1= C(4) TO C(6) TO O(2) 
ANGL 117,1= C(4) TO C(6) TO O(3) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = O(1) TO C(1) 
VIBR .0, 0.00200 = O(1) TO C(7) 
VIBR .0, 0.00500 = C(7) TO C(1) 
VIBR .0, 0.00200 = O(2) TO C(6) 
VIBR .0, 0.00200 = O(3) TO C(6) 
VIBR .0, 0.00200 = C(1) TO C(2) 
VIBR .0, 0.00500 = O(1,5) TO O(1) 
VIBR .0, 0.00500 = C(2) TO O(1) 
VIBR .0, 0.00500 = C(2) TO O(1,5) 
VIBR .0, 0.00200 = C(2) TO C(3,5) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00500 = C(3,5) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(3,5) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00200 = C(4) TO C(5) 
VIBR .0, 0.00200 = C(4) TO C(6) 
VIBR .0, 0.00500 = C(5) TO C(3) 
VIBR .0, 0.00500 = C(6) TO C(3) 
VIBR .0, 0.00500 = C(6) TO C(5) 
VIBR .0, 0.00500 = C(4,5) TO C(4) 
VIBR .0, 0.00500 = O(3) TO C(4) 
VIBR .0, 0.00500 = O(2) TO C(4) 
VIBR .0, 0.00500 = O(2) TO O(3) 
VIBR .0, 0.00200 = C(7) TO C(7,-6,1,0,0,3) 
VIBR .0, 0.00500 = C(7,-6,1,0,0,3) TO O(1) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = O(1) TO C(1) 
U(IJ) .0, 0.04000 = O(1) TO C(7) 
U(IJ) .0, 0.08000 = O(2) TO C(6) 
U(IJ) .0, 0.08000 = O(3) TO C(6) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.04000 = C(2) TO C(3,5) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(4) TO C(5) 
U(IJ) .0, 0.04000 = C(4) TO C(6) 
U(IJ) .0, 0.04000 = C(7) TO C(7,-6,1,0,0,3) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
   0   1   0  x   .
  -1   2   0  x   .
   0   3   0  x   .
  -9  17   4  x   .
 -10  17   4  x   .
  -9  20   1  x   .
  -1   6   7  x   .
  -1   1   1  x   .
  -1   1   2  x   .
  -3  14   1  x   .
   0   4   1  x   .
 -11  20   1  x   .
 -10  20   1  x   .


#===END

data_ST1008
_audit_creation_date        "13-04-29"
_audit_creation_method CRYSTALS_ver_14.40

_oxford_structure_analysis_title  'st2007 in P-3m1'
_chemical_name_systematic         ?
_chemical_melting_point           ?

#looking for refcif 
 
_publ_contact_author_name         'Scott C. McKellar' 
_publ_contact_author_address 
; 
 Dr Scott C. McKellar 
 The University of Edinburgh 
 Joseph Black Building 
 West Mains Road 
 Edinburgh 
 EH9 3JJ 
; 
 
_publ_contact_author_phone        '+44(0)131 6504804' 
_publ_contact_author_email        'smckella@staffmail.ed.ac.uk' 
;

==============================================================================
>>> The Following Model ALERTS were generated                 - (Acta-Mode) <<<
#==============================================================================
    
 
027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............      17.42 Deg.
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low .......       0.93
022_ALERT_3_B Ratio Unique / Expected Reflections (too) Low ..       0.88
023_ALERT_3_B Resolution (too) Low [sin(theta)/Lambda < 0.6]..      23.22 Deg.
088_ALERT_3_B Poor Data / Parameter Ratio ....................       6.33
911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L=  0.555        130
910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) .....          3
913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....         22
341_ALERT_3_C Low Bond Precision on  C-C Bonds (x 1000) Ang ..         12
960_ALERT_3_G Number of Intensities with I .LT. - 2*sig(I) ..           1
950_ALERT_5_G Reported and Calculated Hmax Values Differ by ..          5

The high pressure cell causes shading of a significant proportion of the
sphere of reflections. This means that the completeness is reduced and as
such the quality of the model is lower.All of the above are cause by shading 
by the pressure cell.


601_ALERT_2_A Structure Contains Solvent Accessible VOIDS of .        208 A**3

Structure is a porous framework with disordered solvent in the pores.
The solvent region was treated by the van der Sluis and Spek method, accounting
for 131 e/cell. See below. This corresponds to 2.5 molecules of water  in the 
large pore and 2 molecules of water in each small pore, per formula unit. 
F(000), M, mu, D and the given formulae have been calculated on this assumption.



042_ALERT_1_C Calc. and Reported MoietyFormula Strings  Differ          ?

This is due to the disordered water present in the framework pores. The 
solvent was not able to be modelled and thus was handled using SQUEEZE 
as outlined above. 


045_ALERT_1_C Calculated and Reported Z Differ by ............       3.00 Ratio

This reflects the choice of forumla unit.


152_ALERT_1_C The Supplied and Calc. Volume s.u. Differ by ...         10 Units


This is due to rounding errors.

242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        Cu1

Cu1 is a heavy atom 


220_ALERT_2_C Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       3.13 Ratio

This is caused by C7 which is disordered and subject to thermal motion.
Half occupied carbon refined anistropically.


250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.45

This is probably due to the lack of information in one direction which occurs
as a result of the Merrill-Bassett diamond-anvil cell shading a significant
region of reciprocal space. The effect of this shading is often to cause a
smearing out of electron density in one particular direction.


004_ALERT_5_G Info: Polymeric Structure Found with Dimension .          1
760_ALERT_1_G CIF Contains no Torsion Angles .................          ?

No action taken

779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #         39
              H71  -C7   -H71     8.557   1.555   1.555             40.20 Deg.

Not a genuine bond. C7 is disorderd over 2 sites


301_ALERT_3_G Note: Main Residue  Disorder ...................          5 Perc.

Ester groups are disordered over two sites.


808_ALERT_5_G No Parseable SHELXL Style Weighting Scheme Found          !

A Shelx weighting scheme was not used.


860_ALERT_3_G Note: Number of Least-Squares Restraints .......        116

Thermal similarity, vibration, distance and angle restraints required due 
to disorder and low completeness. 


929_ALERT_5_G No Weight Pars,Obs and Calc R1,wR2,S not checked          !

These have been included
#============================================================================== 

;

loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000 -0.054       217        47 ' '
   2  0.333  0.667  0.000       147        42 ' '
   3  0.667  0.333 -0.064       147        42 ' '
_platon_squeeze_details
;
See above for details.
;
 
_publ_section_exptl_refinement 
; 
; 
 
_publ_section_exptl_prep 
# Brief details or a reference. Include solvent if known 
; 
? 
; 
 
#end of refcif 
_cell_length_a                    18.623(2)
_cell_length_b                    18.623(2)
_cell_length_c                    6.8973(7)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      2071.5(4)
 
_symmetry_cell_setting            'trigonal' 
_symmetry_space_group_name_H-M    'P -3 m 1 ' 
_symmetry_space_group_name_Hall   '-P 3 2' 
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 '-x,-y,-z'
 '-y,x-y,z'
 'y,-x+y,-z'
 '-x+y,-x,z'
 'x-y,x,-z'
 '-x+y,y,z'
 'x-y,-y,-z'
 'x,x-y,z'
 '-x,-x+y,-z'
 '-y,-x,z'
 'y,x,-z'

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source  
 C       0.0033   0.0016   2.3100  20.8439   1.0200  10.2075   1.5886   0.5687
   0.8650  51.6512   0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 H       0.0000   0.0000   0.4930  10.5109   0.3229  26.1257   0.1402   3.1424
   0.0408  57.7998   0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 Cu      0.3201   1.2651  13.3380   3.5828   7.1676   0.2470   5.6158  11.3966
   1.6735  64.8126   1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 O       0.0106   0.0060   3.0485  13.2771   2.2868   5.7011   1.5463   0.3239
   0.8670  32.9089   0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 
 
_cell_formula_units_Z                    2

# Given Formula = C30 H37 Cu3 O27.50 
# Dc =      1.65 Fooo =    906.00 Mu =     16.22 M =    171.37
# Found Formula = C30 H24 Cu3 O21 
# Dc =      1.45 FOOO =    906.00 Mu =     16.01 M =    150.85

_chemical_formula_sum             'C30 H37 Cu3 O27.50'
_chemical_formula_moiety          'C30 H24 Cu3 O21.8.5(H2O)'
_chemical_compound_source                ?
_chemical_formula_weight            1028.24
 
 
_cell_measurement_reflns_used         1241
_cell_measurement_theta_min              3
_cell_measurement_theta_max             23
_cell_measurement_temperature          298
 
_exptl_crystal_description        'block' 
_exptl_crystal_colour             'blue' 
_exptl_crystal_size_min           0.050 
_exptl_crystal_size_mid           0.100 
_exptl_crystal_size_max           0.200 
 
_exptl_crystal_density_diffrn     1.648 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              1048.00 
_exptl_absorpt_coefficient_mu     1.62
 
# Sheldrick geometric approximatio 0.85 0.92 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'SADABS (Siemens, 1996)' 
_exptl_absorpt_correction_T_min   0.77 
_exptl_absorpt_correction_T_max   0.92 
_diffrn_measurement_device_type   'Bruker Kappa Apex2' 
_diffrn_measurement_device        'Area' 
_diffrn_radiation_monochromator   'graphite' 
_diffrn_radiation_type            'Mo K\a'
_diffrn_radiation_wavelength           0.71073
_diffrn_measurement_method        ω/2θ 
 
# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection        'Apex2 (Bruker AXS, 2006)' 
_computing_cell_refinement        'Apex2 (Bruker AXS, 2006)' 
_computing_data_reduction         'Apex2 (Bruker AXS, 2006)' 
_computing_structure_solution     'SIR92 (Altomare et al., 1994)' 
_computing_structure_refinement   'CRYSTALS (Betteridge et al., 2003)' 
_computing_publication_material   'CRYSTALS (Betteridge et al., 2003)' 
_computing_molecular_graphics     'CAMERON (Watkin et al., 1996)' 
 
_diffrn_standards_interval_time   . 
_diffrn_standards_interval_count  . 
_diffrn_standards_number          0 
_diffrn_standards_decay_%         ? 
 
_diffrn_ambient_temperature        298
_diffrn_ambient_pressure 	  0.1 #GPa 	
_diffrn_reflns_number             7248 
_reflns_number_total              974 
_diffrn_reflns_av_R_equivalents   0.099 
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 974 
# Theoretical number of reflections is about 1973 
 
 
_diffrn_reflns_theta_min          2.953 
_diffrn_reflns_theta_max          23.222 
_diffrn_measured_fraction_theta_max 0.882 
 
_diffrn_reflns_theta_full         17.416 
_diffrn_measured_fraction_theta_full 0.925 
 
 
_diffrn_reflns_limit_h_min        -15 
_diffrn_reflns_limit_h_max        0 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        20 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        7 
_reflns_limit_h_min               -15 
_reflns_limit_h_max               0 
_reflns_limit_k_min               0 
_reflns_limit_k_max               20 
_reflns_limit_l_min               0 
_reflns_limit_l_max               7 
 
_oxford_diffrn_Wilson_B_factor    1.24 
_oxford_diffrn_Wilson_scale       49.06 
 
_atom_sites_solution_primary      direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    difmap
 
_refine_diff_density_min          -0.60 
_refine_diff_density_max          0.62 
 
 
# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 
 
 
# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref     I>2.0\s(I)
_refine_ls_number_reflns          595 
_refine_ls_number_restraints      116 
_refine_ls_number_parameters      94 
_oxford_refine_ls_R_factor_ref    0.0630 
_refine_ls_wR_factor_ref          0.0715 
_refine_ls_goodness_of_fit_ref    1.1183 
_refine_ls_shift/su_max           0.0004248 
_refine_ls_shift/su_mean          0.0000439 
 
 
# The values computed with all filters except I/sigma 
_oxford_reflns_number_all         963 
_refine_ls_R_factor_all           0.1365 
_refine_ls_wR_factor_all          0.1262 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0σ(I)
_reflns_number_gt                 595 
_refine_ls_R_factor_gt            0.0630 
_refine_ls_wR_factor_gt           0.0715 
 
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration  '.' 
 
 
_refine_ls_structure_factor_coef  F 
_refine_ls_matrix_type            full
_refine_ls_hydrogen_treatment     noref          #undef, noref, refall,
                                                 # refxyz, refU, constr or mixed
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
;
 Method= Modified Sheldrick 
 w=1/[σ²(F) + ( 0.00P)² + 0.13P] 
 ,where P=(max(Fo,0) + 2Fc)/3 
;
# Insert your own references if required - in alphabetical order 
_publ_section_references 
; 
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., 
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. 
 
Betteridge, P.W., Carruthers, J.R., Cooper, R.I., 
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 
 
Bruker Analytical X-ray Systems, Inc., 2006. Apex2, 
Version 2 User Manual, M86-E01078, Madison, WI. 
 
Siemens Industrial Automation, Inc (1996). 
SADABS: Area-Detector Absorption Correction;: Madison, WI. 
 
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical 
Crystallography Laboratory, Oxford, UK. 
; 

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cu1 Cu 0.47677(5) 0.52323(5) 0.1554(2) 0.0235 1.0000 Uani DS T . . . . 
O1 O 0.4426(4) 0.4113(4) 0.2482(8) 0.0419 1.0000 Uani D U . . . . 
O2 O 0.4809(4) 0.3720(4) -0.0188(8) 0.0415 1.0000 Uani D U . . . . 
O3 O 0.4376(3) 0.5624(3) 0.4115(10) 0.0464 1.0000 Uani DS T . . . . 
O4 O 0.2827(5) 0.0813(5) 0.7412(10) 0.0881 1.0000 Uani D U . . . . 
C1 C 0.4494(5) 0.3586(5) 0.1476(10) 0.0301 1.0000 Uani D U . . . . 
C2 C 0.4218(4) 0.2757(5) 0.2368(10) 0.0312 1.0000 Uani D U . . . . 
C3 C 0.3761(5) 0.2523(5) 0.4070(11) 0.0317 1.0000 Uani D U . . . . 
C4 C 0.3523(5) 0.1762(3) 0.4872(14) 0.0344 1.0000 Uani DS TU . . . . 
C5 C 0.4429(6) 0.2215(3) 0.1512(14) 0.0295 1.0000 Uani DS TU . . . . 
C6 C 0.3029(6) 0.1514(3) 0.6704(15) 0.0551 1.0000 Uani DS TU . . . . 
C7 C 0.2356(8) 0.0485(11) 0.914(2) 0.0928 0.5000 Uani D U . . . . 
H31 H 0.3610 0.2898 0.4718 0.0405 1.0000 Uiso . . . . . . 
H51 H 0.4735 0.2367 0.0294 0.0332 1.0000 Uiso . . . . . . 
H71 H 0.2302 -0.0069 0.9432 0.1047 0.5000 Uiso D . . . . . 
H72 H 0.2626 0.0814 1.0263 0.1047 0.5000 Uiso D . . . . . 
H73 H 0.1814 0.0392 0.9056 0.1047 0.5000 Uiso D . . . . . 
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0274(9) 0.0274(9) 0.0208(8) -0.0006(4) 0.0006(4) 0.0175(11) 
O1 0.071(6) 0.033(4) 0.030(3) 0.015(3) 0.023(4) 0.032(5) 
O2 0.067(6) 0.037(5) 0.031(3) 0.009(3) 0.015(3) 0.034(4) 
O3 0.065(6) 0.065(6) 0.023(5) -0.004(2) 0.004(2) 0.044(7) 
O4 0.136(9) 0.069(6) 0.079(5) 0.044(4) 0.066(5) 0.065(7) 
C1 0.033(7) 0.035(5) 0.031(4) 0.006(3) 0.006(4) 0.023(6) 
C2 0.037(7) 0.034(5) 0.033(4) 0.005(3) 0.003(4) 0.026(5) 
C3 0.040(7) 0.029(5) 0.034(4) 0.000(4) 0.005(4) 0.024(5) 
C4 0.029(9) 0.027(4) 0.047(6) 0.006(3) 0.012(5) 0.015(5) 
C5 0.035(9) 0.029(4) 0.027(6) 0.003(3) 0.006(6) 0.017(5) 
C6 0.083(12) 0.049(5) 0.045(7) 0.013(3) 0.027(6) 0.041(6) 
C7 0.11(2) 0.097(19) 0.051(12) 0.036(12) 0.029(11) 0.033(19) 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 0.1579(9) 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
Cu1 . O1 11_665 1.958(6)    yes
Cu1 . O2 2_665 1.943(6)    yes
Cu1 . O2 12_555 1.943(6)    yes
Cu1 . Cu1 2_665 2.615(3)    yes
Cu1 . O1 . 1.958(6)    yes
Cu1 . O3 . 2.173(8)    yes
O1 . C1 . 1.258(9)    yes
O2 . C1 . 1.255(9)    yes
O4 . C6 . 1.263(9)    yes
O4 . C7 . 1.424(19)    yes
C1 . C2 . 1.495(10)    yes
C2 . C3 . 1.385(10)    yes
C2 . C5 . 1.386(9)    yes
C3 . C4 . 1.373(10)    yes
C3 . H31 . 0.982    no
C4 . C6 . 1.494(15)    yes
C5 . H51 . 0.974    no
C7 . H71 8_557 1.261    no
C7 . H71 . 1.006    no
C7 . H72 . 0.958    no
C7 . H73 . 0.936    no
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
O1 11_665 Cu1 . O2 2_665 90.0(3)    yes
O1 11_665 Cu1 . O2 12_555 168.5(2)    yes
O2 2_665 Cu1 . O2 12_555 89.6(4)    yes
O1 11_665 Cu1 . Cu1 2_665 84.31(17)    yes
O2 2_665 Cu1 . Cu1 2_665 84.23(18)    yes
O2 12_555 Cu1 . Cu1 2_665 84.23(18)    yes
O1 11_665 Cu1 . O1 . 88.0(4)    yes
O2 2_665 Cu1 . O1 . 168.5(2)    yes
O2 12_555 Cu1 . O1 . 90.0(3)    yes
Cu1 2_665 Cu1 . O1 . 84.31(17)    yes
O1 11_665 Cu1 . O3 . 96.1(2)    yes
O2 2_665 Cu1 . O3 . 95.3(2)    yes
O2 12_555 Cu1 . O3 . 95.3(2)    yes
Cu1 2_665 Cu1 . O3 . 179.4(3)    yes
O1 . Cu1 . O3 . 96.1(2)    yes
Cu1 . O1 . C1 . 122.9(5)    yes
Cu1 2_665 O2 . C1 . 123.9(5)    yes
C6 . O4 . C7 . 124.6(7)    yes
O1 . C1 . O2 . 124.6(7)    yes
O1 . C1 . C2 . 117.5(6)    yes
O2 . C1 . C2 . 117.8(6)    yes
C1 . C2 . C3 . 120.9(6)    yes
C1 . C2 . C5 . 120.0(5)    yes
C3 . C2 . C5 . 119.0(6)    yes
C2 . C3 . C4 . 119.8(6)    yes
C2 . C3 . H31 . 120.7    no
C4 . C3 . H31 . 119.5    no
C3 . C4 . C3 9_555 121.3(9)    yes
C3 . C4 . C6 . 119.3(4)    yes
C3 9_555 C4 . C6 . 119.3(4)    yes
C2 . C5 . C2 9_555 121.0(8)    yes
C2 . C5 . H51 . 119.5    no
C2 9_555 C5 . H51 . 119.5    no
C4 . C6 . O4 9_555 117.7(5)    yes
C4 . C6 . O4 . 117.7(5)    yes
O4 9_555 C6 . O4 . 124.6(10)    yes
O4 . C7 . H71 8_557 135.9    no
O4 . C7 . H71 . 109.3    no
H71 8_557 C7 . H71 . 40.2    no
O4 . C7 . H72 . 112.9    no
H71 8_557 C7 . H72 . 66.2    no
H71 . C7 . H72 . 104.3    no
O4 . C7 . H73 . 113.7    no
H71 8_557 C7 . H73 . 106.7    no
H71 . C7 . H73 . 106.0    no
H72 . C7 . H73 . 110.0    no
C7 . H71 . C7 8_557 119.5    no
loop_
 _geom_hbond_atom_site_label_D
 _geom_hbond_site_symmetry_D
 _geom_hbond_atom_site_label_H
 _geom_hbond_site_symmetry_H
 _geom_hbond_atom_site_label_A
 _geom_hbond_site_symmetry_A
 _geom_hbond_angle_DHA
 _geom_hbond_distance_DH
 _geom_hbond_distance_HA
 _geom_hbond_distance_DA
 _geom_hbond_publ_flag
C7 . H71 . O4 8_557 128.9(10) 1.006 2.490 3.218(14)    yes


_iucr_refine_instruction_details_constraints
;
#
# Punched on 29/04/13 at 17:29:38
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
END                                                                             
;


_iucr_refine_instruction_details_restraints
;
#
# Punched on 29/04/13 at 17:29:38
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = O(1) TO C(1) 
VIBR .0, 0.00200 = C(1) TO O(2) 
VIBR .0, 0.00200 = C(1) TO C(2) 
VIBR .0, 0.00500 = O(2) TO O(1) 
VIBR .0, 0.00500 = C(2) TO O(1) 
VIBR .0, 0.00500 = C(2) TO O(2) 
VIBR .0, 0.00200 = C(2) TO C(5) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00500 = C(5) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(5) 
VIBR .0, 0.00500 = C(2,5) TO C(2) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00200 = C(4) TO C(6) 
VIBR .0, 0.00500 = C(3,5) TO C(3) 
VIBR .0, 0.00500 = C(6) TO C(3) 
VIBR .0, 0.00500 = C(6) TO C(3,5) 
VIBR .0, 0.00200 = C(6) TO O(4,5) 
VIBR .0, 0.00200 = C(6) TO O(4) 
VIBR .0, 0.00500 = O(4,5) TO C(4) 
VIBR .0, 0.00500 = O(4) TO C(4) 
VIBR .0, 0.00500 = O(4) TO O(4,5) 
VIBR .0, 0.00200 = O(4) TO C(7) 
VIBR .0, 0.00500 = C(7) TO C(6) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.08000 = O(1) TO C(1) 
U(IJ) .0, 0.08000 = C(1) TO O(2) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.04000 = C(2) TO C(5) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(4) TO C(6) 
U(IJ) .0, 0.04000 = C(6) TO O(4,5) 
U(IJ) .0, 0.04000 = C(6) TO O(4) 
U(IJ) .0, 0.08000 = O(4) TO C(7) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
DISTANCE 2.150000 , 0.050000 = CU(1) TO O(3) 
DISTANCE 1.950000 , 0.050000 = CU(1) TO O(1) 
DISTANCE 1.250000 , 0.050000 = O(1) TO C(1) 
DISTANCE 1.250000 , 0.050000 = C(1) TO O(2) 
DISTANCE 1.490000 , 0.050000 = C(1) TO C(2) 
DISTANCE 1.400000 , 0.050000 = C(2) TO C(5) 
DISTANCE 1.400000 , 0.050000 = C(2) TO C(3) 
DISTANCE 1.400000 , 0.050000 = C(3) TO C(4) 
DISTANCE 1.510000 , 0.050000 = C(4) TO C(6) 
DISTANCE 1.260000 , 0.050000 = C(6) TO O(4) 
DISTANCE 1.430000 , 0.050000 = O(4) TO C(7) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(71) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(72) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(73) 
ANGLE 94.800000 , 1.000000 = O(3) TO CU(1) TO O(1) 
ANGLE 123.000000 , 1.000000 = CU(1) TO O(1) TO C(1) 
ANGLE 120.000000 , 1.000000 = C(1) TO C(2) TO C(5) 
ANGLE 120.000000 , 1.000000 = C(5) TO C(2) TO C(3) 
ANGLE 120.000000 , 1.000000 = C(2) TO C(3) TO C(4) 
ANGLE 120.000000 , 1.000000 = C(3) TO C(4) TO C(6) 
ANGLE 118.000000 , 1.000000 = C(4) TO C(6) TO O(4) 
ANGLE 124.000000 , 1.000000 = C(6) TO O(4) TO C(7) 
ANGLE 118.000000 , 1.000000 = O(2) TO C(1) TO C(2) 
PLANAR 0.010000  C(1) C(2) C(5) C(3) C(4) C(6) O(4) C(7) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
  -1  11   6  x   .
  -3  11   6  x   .
   0   9   5  x   .

#===END

data_ST1009 
_audit_creation_date        "13-05-10"
_audit_creation_method CRYSTALS_ver_14.40

_oxford_structure_analysis_title  'st2016 in P-3m1'
_chemical_name_systematic         ?
_chemical_melting_point           ?

#looking for refcif 
 
_publ_contact_author_name         'Scott C. McKellar' 
_publ_contact_author_address 
; 
 Dr Scott C. McKellar 
 The University of Edinburgh 
 Joseph Black Building 
 West Mains Road 
 Edinburgh 
 EH9 3JJ 
; 
 
_publ_contact_author_phone        '+44(0)131 6504804' 
_publ_contact_author_email        'smckella@staffmail.ed.ac.uk' 
;

#==============================================================================
>>> The Following Model ALERTS were generated                 - (Acta-Mode) <<<
 
022_ALERT_3_A Ratio Unique / Expected Reflections (too) Low ..       0.77
023_ALERT_3_A Resolution (too) Low [sin(theta)/Lambda < 0.6]..      20.82 Deg.
027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............      15.61 Deg.
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low .......       0.82
088_ALERT_3_A Poor Data / Parameter Ratio ....................       4.49
341_ALERT_3_B Low Bond Precision on  C-C Bonds (x 1000) Ang ..         21
911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L=  0.500        173
910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) .....          4
913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....         61
909_ALERT_3_G Percentage of Observed Data at Theta(Max) still          56 Perc.
950_ALERT_5_G Reported and Calculated Hmax Values Differ by ..          5

The high pressure cell causes shading of a significant proportion of the
sphere of reflections. This means that the completeness is reduced and as
such the quality of the model is lower.All of the above are caused by shading 
by the pressure cell.


601_ALERT_2_A Structure Contains Solvent Accessible VOIDS of .        256 A**3

Structure is a porous framework with disordered solvent in the pores.
The solvent region was treated by the van der Sluis and Spek method, accounting
for 118 e/cell. See below. This corresponds to 1.5 molecules of acetonitrile in 
the large pore and 0.5 molecules of acetnoitrle in each small pore, per formula 
unit. F(000), M, mu, D and the given formulae have been calculated on this 
assumption.


201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) .......          1
301_ALERT_3_G Note: Main Residue  Disorder ...................         15 Perc.

There is disordered ligands coordinated to each copper atom which cannot be 
modelled anisotropically. Each coordination site is part-occupied by 
acetonitrile (one third) and water (two thirds).


420_ALERT_2_B D-H Without Acceptor      >O3     -  >H101   ...          ?

This is an O-H bond from coordinated water lying on a mirror plane.


041_ALERT_1_C Calc. and Reported SumFormula    Strings  Differ          ?
042_ALERT_1_C Calc. and Reported MoietyFormula Strings  Differ          ?

This is due to solvent treated with PLATON SQUEEZE


152_ALERT_1_C The Supplied and Calc. Volume s.u. Differ by ...          7 Units

This is due to rounding errors.

220_ALERT_2_C Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       3.62 Ratio

This is unsurprising given the coordinated, disorered solvent and disordered 
ester groups.


242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        Cu1

Cu1 is a heavy atom


250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.12


This is probably due to the lack of information in one direction which occurs
as a result of the Merrill-Bassett diamond-anvil cell shading a significant
region of reciprocal space. The effect of this shading is often to cause a
smearing out of electron density in one particular direction.


860_ALERT_3_G Note: Number of Least-Squares Restraints .......        104

Thermal similarity, vibration, distance and angle restraints required due to 
disorder and low completeness. 



004_ALERT_5_G Info: Polymeric Structure Found with Dimension .          1
760_ALERT_1_G CIF Contains no Torsion Angles .................          ?
811_ALERT_5_G No ADDSYM Analysis: Too Many Excluded Atoms ....          !

NO action taken


779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #         48
              H71  -C7   -H71     9.555   1.555   1.555             39.70 Deg.
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #         63
              C9   -C9   -H92     6.565   1.555  10.665             31.50 Deg.
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #         69
              C9   -C9   -H92     4.565   1.555   1.555             31.50 Deg.

Not genuine bonds. C9 and C7 are disordered over multiple sites.


793_ALERT_4_G The Model has Chirality at C9      (Verify) ....          S

No, this is due to differeing occpuancies of H atoms, one of which is on a 
special position


808_ALERT_5_G No Parseable SHELXL Style Weighting Scheme Found          !

A Shelx weighting scheme was not used.


929_ALERT_5_G No Weight Pars,Obs and Calc R1,wR2,S not checked          !

These have been included.
#==============================================================================

; 

loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000 -0.065       249        68 ' '
   2  0.333  0.667 -0.125        54        25 ' '
   3  0.667  0.333  0.125        54        25 ' '
_platon_squeeze_details 
;
see above for details 
; 
  
_publ_section_exptl_refinement 
; 
; 
 
_publ_section_exptl_prep 
# Brief details or a reference. Include solvent if known 
; 
? 
; 
 
#end of refcif 
_cell_length_a                    18.5488(13)
_cell_length_b                    18.5488(13)
_cell_length_c                    6.9375(4)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      2067.1(2)
 
_symmetry_cell_setting            'trigonal' 
_symmetry_space_group_name_H-M    'P -3 m 1 ' 
_symmetry_space_group_name_Hall   '-P 3 2' 
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 '-x,-y,-z'
 'x-y,x,-z'
 '-x+y,-x,z'
 '-x,-x+y,-z'
 'x,x-y,z'
 '-x+y,y,z'
 'x-y,-y,-z'
 'y,x,-z'
 '-y,-x,z'
 'y,-x+y,-z'
 '-y,x-y,z'

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source  
 C       0.0033   0.0016   2.3100  20.8439   1.0200  10.2075   1.5886   0.5687
   0.8650  51.6512   0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 H       0.0000   0.0000   0.4930  10.5109   0.3229  26.1257   0.1402   3.1424
   0.0408  57.7998   0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 N       0.0061   0.0033  12.2126   0.0057   3.1322   9.8933   2.0125  28.9975
   1.1663   0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 O       0.0106   0.0060   3.0485  13.2771   2.2868   5.7011   1.5463   0.3239
   0.8670  32.9089   0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 Cu      0.3201   1.2651  13.3380   3.5828   7.1676   0.2470   5.6158  11.3966
   1.6735  64.8126   1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 
 
_cell_formula_units_Z                    2

# Given Formula = C37 H32.50 Cu3 N3.50 O20.00 
# Dc =      1.67 Fooo =    941.98 Mu =     16.16 M =    172.80
# Found Formula = C32.00 H25.00 Cu3 N1.00 O20.00 
# Dc =      1.50 FOOO =    941.98 Mu =     16.05 M =    155.69

_chemical_formula_sum             'C37 H32.50 Cu3 N3.50 O20.00'
_chemical_formula_moiety          'C32.00 H25.00 Cu3 N1.00 O20.00.2.5(CH3CN)'
_chemical_compound_source                ?
_chemical_formula_weight            1036.805
 
 
_cell_measurement_reflns_used         1372
_cell_measurement_theta_min              3
_cell_measurement_theta_max             23
_cell_measurement_temperature          298
_diffrn_ambient_pressure    	  0.3 #GPa
 
_exptl_crystal_description        'rod' 
_exptl_crystal_colour             'blue' 
_exptl_crystal_size_min           0.030 
_exptl_crystal_size_mid           0.030 
_exptl_crystal_size_max           0.080 
 
_exptl_crystal_density_diffrn     1.666 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              1052.00 
_exptl_absorpt_coefficient_mu     1.62 
 
# Sheldrick geometric approximatio 0.95 0.95 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'SADABS (Siemens, 1996)' 
_exptl_absorpt_correction_T_min   0.39 
_exptl_absorpt_correction_T_max   0.95 
_diffrn_measurement_device_type   'Bruker Kappa Apex2' 
_diffrn_measurement_device        'Area' 
_diffrn_radiation_monochromator   'graphite' 
_diffrn_radiation_type            'Mo K\a'
_diffrn_radiation_wavelength           0.71073
_diffrn_measurement_method        ω/2θ 
 
# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection        'Apex2 (Bruker AXS, 2006)' 
_computing_cell_refinement        'Apex2 (Bruker AXS, 2006)' 
_computing_data_reduction         'Apex2 (Bruker AXS, 2006)' 
_computing_structure_solution     'SIR92 (Altomare et al., 1994)' 
_computing_structure_refinement   'CRYSTALS (Betteridge et al., 2003)' 
_computing_publication_material   'CRYSTALS (Betteridge et al., 2003)' 
_computing_molecular_graphics     'CAMERON (Watkin et al., 1996)' 
 
_diffrn_standards_interval_time   . 
_diffrn_standards_interval_count  . 
_diffrn_standards_number          0 
_diffrn_standards_decay_%         ? 
 
_diffrn_ambient_temperature        298
_diffrn_reflns_number             6642 
_reflns_number_total              626 
_diffrn_reflns_av_R_equivalents   0.108 
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 626 
# Theoretical number of reflections is about 1443 
 
 
_diffrn_reflns_theta_min          3.199 
_diffrn_reflns_theta_max          20.816 
_diffrn_measured_fraction_theta_max 0.769 
 
_diffrn_reflns_theta_full         15.612 
_diffrn_measured_fraction_theta_full 0.821 
 
 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        0 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        17 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        6 
_reflns_limit_h_min               -13 
_reflns_limit_h_max               0 
_reflns_limit_k_min               0 
_reflns_limit_k_max               17 
_reflns_limit_l_min               0 
_reflns_limit_l_max               6 
 
_oxford_diffrn_Wilson_B_factor    1.60 
_oxford_diffrn_Wilson_scale       129.17 
 
_atom_sites_solution_primary      direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    difmap
 
_refine_diff_density_min          -0.62 
_refine_diff_density_max          0.66 
 
 
# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 
 
 
# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref     I>2.0\s(I)
_refine_ls_number_reflns          449 
_refine_ls_number_restraints      104 
_refine_ls_number_parameters      100 
_oxford_refine_ls_R_factor_ref    0.0558 
_refine_ls_wR_factor_ref          0.0654 
_refine_ls_goodness_of_fit_ref    0.9979 
_refine_ls_shift/su_max           0.0001632 
_refine_ls_shift/su_mean          0.0000079 
 
 
# The values computed with all filters except I/sigma 
_oxford_reflns_number_all         608 
_refine_ls_R_factor_all           0.0835 
_refine_ls_wR_factor_all          0.0994 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0σ(I)
_reflns_number_gt                 449 
_refine_ls_R_factor_gt            0.0558 
_refine_ls_wR_factor_gt           0.0654 
 
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration  '.' 
 
 
_refine_ls_structure_factor_coef  F 
_refine_ls_matrix_type            full
_refine_ls_hydrogen_treatment     noref          #undef, noref, refall,
                                                 # refxyz, refU, constr or mixed
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.723 0.165 0.128 
;
# Insert your own references if required - in alphabetical order 
_publ_section_references 
; 
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., 
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. 
 
Betteridge, P.W., Carruthers, J.R., Cooper, R.I., 
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 
 
Bruker Analytical X-ray Systems, Inc., 2006. Apex2, 
Version 2 User Manual, M86-E01078, Madison, WI. 
 
Prince, E. 
Mathematical Techniques in Crystallography 
and Materials Science 
Springer-Verlag, New York, 1982. 
 
Siemens Industrial Automation, Inc (1996). 
SADABS: Area-Detector Absorption Correction;: Madison, WI. 
 
Watkin D.J. (1994). 
Acta Cryst, A50, 411-437. 
 
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical 
Crystallography Laboratory, Oxford, UK. 
; 

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cu1 Cu 0.47614(7) 0.52386(7) 0.8474(3) 0.0257 1.0000 Uani DS T . . . . 
N1 N 0.4321(10) 0.5679(10) 0.607(4) 0.044(4) 0.3330 Uiso DS U . . . . 
O1 O 0.5883(5) 0.5601(6) 0.7516(10) 0.0435 1.0000 Uani D U . . . . 
O2 O 0.6288(5) 0.5179(6) 1.0131(10) 0.0420 1.0000 Uani . U . . . . 
O3 O 0.4425(6) 0.5575(6) 0.582(2) 0.042(4) 0.6670 Uiso S U . . . . 
O4 O 0.7922(7) 0.7049(8) 0.2350(14) 0.0883 1.0000 Uani . U . . . . 
C1 C 0.6420(8) 0.5507(8) 0.8469(16) 0.0355 1.0000 Uani . U . . . . 
C2 C 0.7241(8) 0.5773(9) 0.7562(14) 0.0348 1.0000 Uani D U . . . . 
C3 C 0.7427(8) 0.6151(8) 0.5801(15) 0.0330 1.0000 Uani D U . . . . 
C4 C 0.8188(6) 0.6377(13) 0.493(2) 0.0423 1.0000 Uani DS TU . . . . 
C5 C 0.7787(6) 0.5573(12) 0.845(2) 0.0294 1.0000 Uani DS TU . . . . 
C6 C 0.8409(7) 0.6819(15) 0.302(3) 0.0579 1.0000 Uani S TU . . . . 
C7 C 0.8036(15) 0.7524(17) 0.076(3) 0.1008 0.5000 Uani D U . . . . 
C8 C 0.4022(10) 0.5978(10) 0.510(4) 0.045(4) 0.3330 Uiso DS U . . . . 
C9 C 0.3628(5) 0.6372(5) 0.397(3) 0.045(5) 0.3330 Uiso DS U . . . . 
H31 H 0.7078 0.6333 0.5228 0.0500 1.0000 Uiso . . . . . . 
H51 H 0.7656 0.5312 0.9706 0.0500 1.0000 Uiso . . . . . . 
H91 H 0.3680 0.6320 0.2540 0.0475 0.3330 Uiso D . . . . . 
H92 H 0.3045 0.6091 0.4285 0.0475 0.6670 Uiso D . . . . . 
H101 H 0.4604 0.5961 0.5838 0.0500 0.6670 Uiso . . . . . . 
H71 H 0.7571 0.7609 0.0568 0.1172 0.5000 Uiso D . . . . . 
H72 H 0.8526 0.8064 0.0897 0.1172 0.5000 Uiso D . . . . . 
H73 H 0.8101 0.7270 -0.0374 0.1172 0.5000 Uiso D . . . . . 
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0282(12) 0.0282(12) 0.0261(11) 0.0000(5) 0.0000(5) 0.0180(13) 
O1 0.035(6) 0.053(7) 0.041(4) 0.012(4) 0.007(4) 0.020(6) 
O2 0.028(6) 0.059(7) 0.041(4) 0.008(4) 0.004(3) 0.023(5) 
O4 0.078(9) 0.119(11) 0.079(6) 0.053(6) 0.006(6) 0.058(8) 
C1 0.032(6) 0.034(9) 0.037(5) -0.002(5) 0.002(4) 0.014(7) 
C2 0.040(6) 0.040(9) 0.035(5) -0.002(5) 0.004(4) 0.027(7) 
C3 0.025(7) 0.036(9) 0.047(5) 0.010(5) -0.001(4) 0.022(7) 
C4 0.033(6) 0.053(13) 0.048(8) 0.015(7) 0.007(3) 0.027(7) 
C5 0.034(5) 0.029(11) 0.023(7) -0.001(7) 0.000(3) 0.015(6) 
C6 0.057(7) 0.078(14) 0.045(8) 0.019(7) 0.010(4) 0.039(7) 
C7 0.08(3) 0.14(3) 0.063(17) 0.047(17) -0.026(17) 0.03(2) 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 0.1364(10) 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
Cu1 . O1 10_665 1.955(9)    yes
Cu1 . O2 2_667 1.954(8)    yes
Cu1 . O2 9_557 1.954(8)    yes
Cu1 . Cu1 2_667 2.614(4)    yes
Cu1 . N1 . 2.19(4)    yes
Cu1 . O1 . 1.955(9)    yes
Cu1 . O3 . 2.137(19)    yes
N1 . C8 . 1.17(4)    yes
O1 . C1 . 1.279(14)    yes
O2 . C1 . 1.270(13)    yes
O3 . H101 10_665 0.621    no
O3 . H101 . 0.621    no
O4 . C6 . 1.265(12)    yes
O4 . C7 . 1.36(3)    yes
C1 . C2 . 1.485(17)    yes
C2 . C3 . 1.363(14)    yes
C2 . C5 . 1.384(13)    yes
C3 . C4 . 1.394(13)    yes
C3 . H31 . 0.955    no
C4 . C6 . 1.51(3)    yes
C5 . H51 . 0.968    no
C7 . H71 9_555 1.248    no
C7 . H71 . 0.962    no
C7 . H72 . 0.962    no
C7 . H73 . 0.957    no
C8 . C9 . 1.49(4)    yes
C9 . C9 4_565 1.64(3)    yes
C9 . C9 6_565 1.64(3)    yes
C9 . H92 10_665 0.960    no
C9 . H91 . 1.009    no
C9 . H92 . 0.960    no
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
O1 10_665 Cu1 . O2 2_667 90.1(4)    yes
O1 10_665 Cu1 . O2 9_557 169.3(3)    yes
O2 2_667 Cu1 . O2 9_557 88.2(5)    yes
O1 10_665 Cu1 . Cu1 2_667 84.8(2)    yes
O2 2_667 Cu1 . Cu1 2_667 84.5(2)    yes
O2 9_557 Cu1 . Cu1 2_667 84.5(2)    yes
O1 10_665 Cu1 . N1 . 98.3(5)    yes
O2 2_667 Cu1 . N1 . 92.3(5)    yes
O2 9_557 Cu1 . N1 . 92.3(5)    yes
Cu1 2_667 Cu1 . N1 . 175.6(6)    yes
O1 10_665 Cu1 . O1 . 89.5(5)    yes
O2 2_667 Cu1 . O1 . 169.3(3)    yes
O2 9_557 Cu1 . O1 . 90.1(4)    yes
Cu1 2_667 Cu1 . O1 . 84.8(2)    yes
N1 . Cu1 . O1 . 98.3(5)    yes
O1 10_665 Cu1 . O3 . 91.2(4)    yes
O2 2_667 Cu1 . O3 . 99.5(4)    yes
O2 9_557 Cu1 . O3 . 99.5(4)    yes
Cu1 2_667 Cu1 . O3 . 174.5(5)    yes
N1 . Cu1 . O3 . 10.0(8)    yes
O1 . Cu1 . O3 . 91.2(4)    yes
Cu1 . N1 . C8 . 165.5(9)    yes
Cu1 . O1 . C1 . 123.0(7)    yes
Cu1 2_667 O2 . C1 . 123.7(8)    yes
Cu1 . O3 . H101 10_665 104.5    no
Cu1 . O3 . H101 . 104.5    no
H101 10_665 O3 . H101 . 115.1    no
C6 . O4 . C7 . 127.6(16)    yes
O1 . C1 . O2 . 123.9(11)    yes
O1 . C1 . C2 . 118.4(10)    yes
O2 . C1 . C2 . 117.7(12)    yes
C1 . C2 . C3 . 120.3(11)    yes
C1 . C2 . C5 . 119.2(10)    yes
C3 . C2 . C5 . 120.3(12)    yes
C2 . C3 . C4 . 120.1(12)    yes
C2 . C3 . H31 . 120.8    no
C4 . C3 . H31 . 118.5    no
C3 7_655 C4 . C3 . 119.3(15)    yes
C3 7_655 C4 . C6 . 120.3(7)    yes
C3 . C4 . C6 . 120.3(7)    yes
C2 . C5 . C2 7_655 119.8(14)    yes
C2 . C5 . H51 . 120.1    no
C2 7_655 C5 . H51 . 120.1    no
C4 . C6 . O4 . 117.5(9)    yes
C4 . C6 . O4 7_655 117.5(9)    yes
O4 . C6 . O4 7_655 124.1(19)    yes
H71 9_555 C7 . O4 . 138.3    no
H71 9_555 C7 . H71 . 39.7    no
O4 . C7 . H71 . 111.1    no
H71 9_555 C7 . H72 . 107.4    no
O4 . C7 . H72 . 111.0    no
H71 . C7 . H72 . 107.4    no
H71 9_555 C7 . H73 . 70.3    no
O4 . C7 . H73 . 111.5    no
H71 . C7 . H73 . 107.9    no
H72 . C7 . H73 . 107.8    no
N1 . C8 . C9 . 176.4(9)    yes
C8 . C9 . C9 4_565 137.5(4)    yes
C8 . C9 . C9 6_565 137.5(4)    yes
C9 4_565 C9 . C9 6_565 60.000(3)    yes
C8 . C9 . H92 10_665 108.1    no
C9 4_565 C9 . H92 10_665 89.0    no
C9 6_565 C9 . H92 10_665 31.5    no
C8 . C9 . H91 . 112.0    no
C9 4_565 C9 . H91 . 98.3    no
C9 6_565 C9 . H91 . 98.3    no
H92 10_665 C9 . H91 . 107.8    no
C8 . C9 . H92 . 108.1    no
C9 4_565 C9 . H92 . 31.5    no
C9 6_565 C9 . H92 . 89.0    no
H92 10_665 C9 . H92 . 113.2    no
H91 . C9 . H92 . 107.8    no
C9 4_565 H92 . C9 . 117.1    no
C7 . H71 . C7 9_555 124.2    no
loop_
 _geom_hbond_atom_site_label_D
 _geom_hbond_site_symmetry_D
 _geom_hbond_atom_site_label_H
 _geom_hbond_site_symmetry_H
 _geom_hbond_atom_site_label_A
 _geom_hbond_site_symmetry_A
 _geom_hbond_angle_DHA
 _geom_hbond_distance_DH
 _geom_hbond_distance_HA
 _geom_hbond_distance_DA
 _geom_hbond_publ_flag
C9 . H92 . C8 4_565 157.0(11) 0.960 2.007 2.91(2)    yes
C9 4_565 H92 . C8 . 157.0(11) 0.960 2.007 2.91(2)    yes
C7 . H71 . O4 9_555 130.8(14) 0.962 2.436 3.15(2)    yes
C7 . H71 . C7 9_555 124(2) 0.962 1.248 1.96(2)    yes


_iucr_refine_instruction_details_constraints
;
#
# Punched on 10/05/13 at 12:39:47
#
#LIST     12                                                                    
BLOCK 
CONT SCALE 
CONT CU   (    1 ,X'S,U'S) 
CONT N    (    1 ,X'S,U[ISO]) 
CONT O    (    1 ,X'S,U'S)  UNTIL O    (    2 ) 
CONT O    (    3 ,X'S,U[ISO]) 
CONT O    (    4 ,X'S,U'S)  UNTIL C    (    7 ) 
CONT C    (    8 ,X'S,U[ISO])  UNTIL C    (    9 ) 
END                                                                             
;


_iucr_refine_instruction_details_restraints
;
#
# Punched on 10/05/13 at 12:39:47
#
#LIST     16                                                                    
NO 
DISTANCE 1.450000 , 0.050000 = C(9) TO C(8) 
DISTANCE 1.130000 , 0.050000 = N(1) TO C(8) 
DISTANCE 2.180000 , 0.050000 = CU(1) TO N(1) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(71) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(73) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(72) 
DISTANCE 1.400000 , 0.050000 = C(2) TO C(3) 
ANGLE 170.000000 , 1.000000 = CU(1) TO N(1) TO C(8) 
ANGLE 90.000000 , 1.000000 = N(1) TO CU(1) TO O(1) 
ANGLE 180.000000 , 1.000000 = N(1) TO C(8) TO C(9) 
ANGLE 110.000000 , 1.000000 = C(8) TO C(9) TO H(92) 
ANGLE 110.000000 , 1.000000 = C(8) TO C(9) TO H(91) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00500 = O(3) TO N(1) 
VIBR .0, 0.00500 = O(1) TO N(1) 
VIBR .0, 0.00500 = O(1) TO O(3) 
VIBR .0, 0.00200 = N(1) TO C(8) 
VIBR .0, 0.00200 = O(1) TO C(1) 
VIBR .0, 0.00200 = C(1) TO O(2) 
VIBR .0, 0.00200 = C(1) TO C(2) 
VIBR .0, 0.00500 = O(2) TO O(1) 
VIBR .0, 0.00500 = C(2) TO O(1) 
VIBR .0, 0.00500 = C(2) TO O(2) 
VIBR .0, 0.00200 = C(2) TO C(5) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00500 = C(5) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(5) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00200 = C(4) TO C(6) 
VIBR .0, 0.00500 = C(6) TO C(3) 
VIBR .0, 0.00200 = C(6) TO O(4) 
VIBR .0, 0.00500 = O(4) TO C(4) 
VIBR .0, 0.00200 = O(4) TO C(7) 
VIBR .0, 0.00500 = C(7) TO C(6) 
VIBR .0, 0.00200 = C(9) TO C(8) 
VIBR .0, 0.00500 = N(1) TO C(9) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = N(1) TO C(8) 
U(IJ) .0, 0.04000 = O(1) TO C(1) 
U(IJ) .0, 0.04000 = C(1) TO O(2) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.04000 = C(2) TO C(5) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(4) TO C(6) 
U(IJ) .0, 0.04000 = C(6) TO O(4,4,1,1) 
U(IJ) .0, 0.04000 = C(6) TO O(4) 
U(IJ) .0, 0.08000 = O(4) TO C(7) 
U(IJ) .0, 0.08000 = C(9) TO C(8) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(73) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(71) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(72) 
DISTANCE 0.950000 , 0.050000 = C(9) TO H(91) 
DISTANCE 0.950000 , 0.050000 = C(9) TO H(92) 
DISTANCE 1.400000 , 0.050000 = C(2) TO C(5) 
DISTANCE 1.400000 , 0.050000 = C(3) TO C(4) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
 -11  15   1  x   .
  -2  12   0  x   .
 -11  14   1  x   .
 -12  17   2  x   .
 -12  15   1  x   .
   0   9   4  x   .
 -11  13   2  x   .
 -11  16   2  x   .
  -8  17   2  x   .
  -6  14   1  x   .
  -4  15   2  x   .
 -10  11   5  x   .
  -4   8   1  x   .

#===END

data_ST1010 
_audit_creation_date        "12-10-30"
_audit_creation_method CRYSTALS_ver_14.40

_oxford_structure_analysis_title  'ST2019 in P-3m1'
_chemical_name_systematic         ?
_chemical_melting_point           ?

#looking for refcif 
 
_publ_contact_author_name         'Scott C. McKellar' 
_publ_contact_author_address 
; 
 Dr Scott C. McKellar 
 The University of Edinburgh 
 Joseph Black Building 
 West Mains Road 
 Edinburgh 
 EH9 3JJ 
; 
 
_publ_contact_author_phone        '+44(0)131 6504804' 
_publ_contact_author_email        'smckella@staffmail.ed.ac.uk' 
;
 
#==============================================================================
>>> The Following Model ALERTS were generated                 - (Acta-Mode) <<<
#==============================================================================
 
601_ALERT_2_A Structure Contains Solvent Accessible VOIDS of .        228 A**3

Structure is a porous framework with disordered solvent in the pores.
The solvent region was treated by the van der Sluis and Spek method, accounting
for 74 e/cell. See below. This corresponds to 0.5 molecule of water in the small 
pore and 1 molecule of acetonitrle in the large pore, per formula unit.
F(000), M, mu, D and the given formulae have been calculated on this assumption.


201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) .......          1
301_ALERT_3_G Note: Main Residue  Disorder ...................         14 Perc.

There is disordered ligands coordinated to each copper atom which cannot be 
modelled anisotropically. Each coordination site is part-occupied by 
acetonitrile (one third) and water (two thirds). 


420_ALERT_2_B D-H Without Acceptor      >O3     -  >H101   ...          ?

This is an O-H bond from coordinated water lying on a mirror plane.


152_ALERT_1_C The Supplied and Calc. Volume s.u. Differ by ...         20 Units
This is due to rounding errors.


220_ALERT_2_C Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       3.39 Ratio
This is unsurprising given the coordinated, disorered solvent and 
disordered ester groups.

341_ALERT_3_C Low Bond Precision on  C-C Bonds (x 1000) Ang ..         10
This is due to the lack of high angle data and disorder of the 
coordinated ligand.


004_ALERT_5_G Info: Polymeric Structure Found with Dimension .          1

Structure is a coordination polymer.


779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #         48
              H71  -C7   -H71    12.555   1.555   1.555             29.10 Deg.
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #         60
              H92  -C9   -C9      3.665   1.555   3.665             31.90 Deg.
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #         71
              C9   -C9   -H92     5.565   1.555   1.555             31.90 Deg.

Not a genuine bond. C7 and C9 are disordered over multiple sites.


760_ALERT_1_G CIF Contains no Torsion Angles .................          

No action taken.


808_ALERT_5_G No Parseable SHELXL Style Weighting Scheme Found          !

A Shelx weighting scheme was not used.


811_ALERT_5_G No ADDSYM Analysis: Too Many Excluded Atoms ....          !

No action taken.

860_ALERT_3_G Note: Number of Least-Squares Restraints .......         86

Thermal similarity, vibration, distance and angle restraints required due to 
disordered ligands. 


929_ALERT_5_G No Weight Pars,Obs and Calc R1,wR2,S not checked          !
These have been included.

960_ALERT_3_G Number of Intensities with I .LT. - 2*sig(I) ..           1

This is caused by weak data at high angle

950_ALERT_5_G Reported and Calculated Hmax Values Differ by ..          4

This is probably because the data collection was a sphere, not a 
refined strategy. Data is still 100% complete to 26 degrees 
theta as shown below

Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged)

Theta sin(th)/Lambda Complete  Expected Measured  Missing
-------------------------------------------------------------------------------
 20.82     0.500     1.000          810      810        0
 23.01     0.550     0.999         1074     1073        1
 25.24     0.600     1.000         1379     1379        0
------------------------------------------------------------ ACTA Min. Res. ---
 26.39     0.625     1.000         1553     1553        0


250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.57

The use of restraints in the refinement mean that off diagonal terms in the
variance-covariance matrix are significant, and the diagonal approximation
used in Platon/Checkcif is subject to error 
#============================================================================== 
;


loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000 -0.058       225        48 ' '
   2  0.667  0.333  0.108        38        13 ' '
   3  0.333  0.667  0.892        38        13 ' '
_platon_squeeze_details
;
see above for details
;
 
_publ_section_exptl_refinement 
; 
; 
 
_publ_section_exptl_prep 
# Brief details or a reference. Include solvent if known 
; 
? 
; 
 
#end of refcif 
_cell_length_a                    18.5877(5)
_cell_length_b                    18.5877(5)
_cell_length_c                    6.8740(2)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      2056.80(10)
 
_symmetry_cell_setting            'trigonal' 
_symmetry_space_group_name_H-M    'P -3 m 1 ' 
_symmetry_space_group_name_Hall   '-P 3 2' 
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 '-x,-y,-z'
 '-y,x-y,z'
 'y,-x+y,-z'
 '-x+y,-x,z'
 'x-y,x,-z'
 '-x+y,y,z'
 'x-y,-y,-z'
 'x,x-y,z'
 '-x,-x+y,-z'
 '-y,-x,z'
 'y,x,-z'

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source  
 C       0.0033   0.0016   2.3100  20.8439   1.0200  10.2075   1.5886   0.5687
   0.8650  51.6512   0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 H       0.0000   0.0000   0.4930  10.5109   0.3229  26.1257   0.1402   3.1424
   0.0408  57.7998   0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 N       0.0061   0.0033  12.2126   0.0057   3.1322   9.8933   2.0125  28.9975
   1.1663   0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 O       0.0106   0.0060   3.0485  13.2771   2.2868   5.7011   1.5463   0.3239
   0.8670  32.9089   0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 Cu      0.3201   1.2651  13.3380   3.5828   7.1676   0.2470   5.6158  11.3966
   1.6735  64.8126   1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 
 
_cell_formula_units_Z                    2

# Given Formula = C34 H29.00 Cu3 N2.00 O21 
# Dc =      1.60 Fooo =    939.98 Mu =     16.21 M =    165.37
# Found Formula = C32.00 H24 Cu3 N1.00 O20.00 
# Dc =      1.51 FOOO =    939.98 Mu =     16.13 M =    155.53

_chemical_formula_sum             'C35 H31.00 Cu3 N2.50 O21'
_chemical_formula_moiety          'C32.00 H24 Cu3 N1.00 O20.00.1.5(CH3CN)'
_chemical_compound_source                ?
_chemical_formula_weight            992.235
 
 
_cell_measurement_reflns_used         3570
_cell_measurement_theta_min              2
_cell_measurement_theta_max             25
_cell_measurement_temperature          150
 
_exptl_crystal_description        'rod' 
_exptl_crystal_colour             'blue' 
_exptl_crystal_size_min           0.030 
_exptl_crystal_size_mid           0.030 
_exptl_crystal_size_max           0.080 
 
_exptl_crystal_density_diffrn     1.602 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              1004.00 
_exptl_absorpt_coefficient_mu     1.62 
 
# Sheldrick geometric approximatio 0.95 0.95 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'SADABS (Siemens, 1996)' 
_exptl_absorpt_correction_T_min   0.75 
_exptl_absorpt_correction_T_max   0.95 
_diffrn_measurement_device_type   'Bruker Kappa Apex2' 
_diffrn_measurement_device        'Area' 
_diffrn_radiation_monochromator   'graphite' 
_diffrn_radiation_type            'Mo K\a'
_diffrn_radiation_wavelength           0.71073
_diffrn_measurement_method        'φ & ω scans' 
 
# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection        'Apex2 (Bruker AXS, 2006)' 
_computing_cell_refinement        'Apex2 (Bruker AXS, 2006)' 
_computing_data_reduction         'Apex2 (Bruker AXS, 2006)' 
_computing_structure_solution     'SIR92 (Altomare et al., 1994)' 
_computing_structure_refinement   'CRYSTALS (Betteridge et al., 2003)' 
_computing_publication_material   'CRYSTALS (Betteridge et al., 2003)' 
_computing_molecular_graphics     'CAMERON (Watkin et al., 1996)' 
 
_diffrn_standards_interval_time   . 
_diffrn_standards_interval_count  . 
_diffrn_standards_number          0 
_diffrn_standards_decay_%         ? 
 
_diffrn_ambient_temperature        150
_diffrn_reflns_number             20617 
_reflns_number_total              1553 
_diffrn_reflns_av_R_equivalents   0.118 
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 1553 
# Theoretical number of reflections is about 2811 
 
 
_diffrn_reflns_theta_min          1.265 
_diffrn_reflns_theta_max          26.394 
_diffrn_measured_fraction_theta_max 0.999 
 
_diffrn_reflns_theta_full         26.394 
_diffrn_measured_fraction_theta_full 0.999 
 
 
_diffrn_reflns_limit_h_min        -19 
_diffrn_reflns_limit_h_max        0 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        23 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        8 
_reflns_limit_h_min               -19 
_reflns_limit_h_max               0 
_reflns_limit_k_min               0 
_reflns_limit_k_max               23 
_reflns_limit_l_min               0 
_reflns_limit_l_max               8 
 
_oxford_diffrn_Wilson_B_factor    1.07 
_oxford_diffrn_Wilson_scale       111.54 
 
_atom_sites_solution_primary      direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    difmap
 
_refine_diff_density_min          -1.99 
_refine_diff_density_max          1.91 
 
 
# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 
 
 
# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref     I>-10.0\s(I)
_refine_ls_number_reflns          1542 
_refine_ls_number_restraints      86 
_refine_ls_number_parameters      100 
_oxford_refine_ls_R_factor_ref    0.0798 
_refine_ls_wR_factor_ref          0.1599 
_refine_ls_goodness_of_fit_ref    0.9830 
_refine_ls_shift/su_max           0.0004673 
_refine_ls_shift/su_mean          0.0000245 
 
 
# The values computed with all filters except I/sigma 
_oxford_reflns_number_all         1542 
_refine_ls_R_factor_all           0.0798 
_refine_ls_wR_factor_all          0.1599 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0σ(I)
_reflns_number_gt                 1159 
_refine_ls_R_factor_gt            0.0574 
_refine_ls_wR_factor_gt           0.1529 
 
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration  '.' 
 
 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full
_refine_ls_hydrogen_treatment     noref          #undef, noref, refall,
                                                 # refxyz, refU, constr or mixed
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.07P)² +15.03P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
# Insert your own references if required - in alphabetical order 
_publ_section_references 
; 
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., 
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. 
 
Betteridge, P.W., Carruthers, J.R., Cooper, R.I., 
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 
 
Bruker Analytical X-ray Systems, Inc., 2006. Apex2, 
Version 2 User Manual, M86-E01078, Madison, WI. 
 
Siemens Industrial Automation, Inc (1996). 
SADABS: Area-Detector Absorption Correction;: Madison, WI. 
 
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical 
Crystallography Laboratory, Oxford, UK. 
; 

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cu1 Cu 0.47648(3) 0.52352(3) 0.84513(12) 0.0151 1.0000 Uani DS T . . . . 
N1 N 0.4341(6) 0.5659(6) 0.606(3) 0.032(2) 0.3330 Uiso DS U . . . . 
O1 O 0.5886(2) 0.5585(3) 0.7514(6) 0.0331 1.0000 Uani D U . . . . 
O2 O 0.6286(3) 0.5186(3) 1.0177(5) 0.0360 1.0000 Uani . U . . . . 
O3 O 0.4417(3) 0.5583(3) 0.5783(13) 0.0230(16) 0.6670 Uiso DS U . . . . 
O4 O 0.7962(4) 0.7123(4) 0.2433(8) 0.0624 1.0000 Uani . U . . . . 
C1 C 0.6411(3) 0.5502(3) 0.8498(7) 0.0217 1.0000 Uani . U . . . . 
C2 C 0.7234(3) 0.5767(4) 0.7581(7) 0.0216 1.0000 Uani . U . . . . 
C3 C 0.7457(4) 0.6199(4) 0.5842(8) 0.0267 1.0000 Uani . U . . . . 
C4 C 0.8214(3) 0.6427(6) 0.4987(12) 0.0310 1.0000 Uani S TU . . . . 
C5 C 0.7786(3) 0.5573(5) 0.8482(11) 0.0221 1.0000 Uani S TU . . . . 
C6 C 0.8465(3) 0.6930(6) 0.3132(14) 0.0411 1.0000 Uani S TU . . . . 
C7 C 0.8122(13) 0.7590(14) 0.076(2) 0.0739 0.5000 Uani D U . . . . 
C8 C 0.4052(7) 0.5948(7) 0.513(3) 0.040(3) 0.3330 Uiso DS U . . . . 
C9 C 0.3637(4) 0.6363(4) 0.401(3) 0.043(3) 0.3330 Uiso DS U . . . . 
H31 H 0.7079 0.6334 0.5232 0.0500 1.0000 Uiso . . . . . . 
H51 H 0.7656 0.5313 0.9701 0.0500 1.0000 Uiso . . . . . . 
H71 H 0.7667 0.7678 0.0440 0.0889 0.5000 Uiso . . . . . . 
H72 H 0.8610 0.8128 0.0902 0.0889 0.5000 Uiso . . . . . . 
H73 H 0.8210 0.7322 -0.0335 0.0889 0.5000 Uiso D . . . . . 
H91 H 0.3680 0.6320 0.2690 0.0475 0.3330 Uiso D . . . . . 
H92 H 0.3045 0.6091 0.4435 0.0475 0.3330 Uiso D . . . . . 
H101 H 0.4603 0.5962 0.5825 0.0500 0.6670 Uiso D . . . . . 
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0181(4) 0.0181(4) 0.0137(4) -0.00050(17) 0.00050(17) 0.0125(4) 
O1 0.024(2) 0.053(3) 0.027(2) 0.0149(19) 0.0066(16) 0.022(2) 
O2 0.028(2) 0.065(3) 0.0236(19) 0.0138(19) 0.0042(17) 0.031(2) 
O4 0.055(3) 0.090(4) 0.055(3) 0.045(3) 0.013(3) 0.046(3) 
C1 0.022(3) 0.023(3) 0.024(3) 0.000(2) 0.001(2) 0.014(2) 
C2 0.020(3) 0.026(3) 0.023(2) 0.001(2) 0.000(2) 0.014(2) 
C3 0.023(3) 0.033(3) 0.030(3) 0.008(2) 0.006(2) 0.019(3) 
C4 0.030(3) 0.047(5) 0.022(4) 0.015(4) 0.0075(18) 0.023(3) 
C5 0.022(3) 0.025(4) 0.020(4) 0.000(3) -0.0001(15) 0.013(2) 
C6 0.035(4) 0.049(6) 0.044(5) 0.026(4) 0.013(2) 0.025(3) 
C7 0.084(14) 0.103(16) 0.045(9) 0.019(9) -0.008(9) 0.055(12) 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 0.14163(18) 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
Cu1 . O1 11_665 1.957(4)    yes
Cu1 . O2 2_667 1.946(4)    yes
Cu1 . O2 12_557 1.946(4)    yes
Cu1 . Cu1 2_667 2.6128(17)    yes
Cu1 . N1 . 2.13(2)    yes
Cu1 . O1 . 1.957(4)    yes
Cu1 . O3 . 2.148(10)    yes
N1 . C8 . 1.13(3)    yes
O1 . C1 . 1.259(7)    yes
O2 . C1 . 1.263(6)    yes
O3 . H101 11_665 0.611    no
O3 . H101 . 0.611    no
O4 . C6 . 1.253(6)    yes
O4 . C7 . 1.381(16)    yes
C1 . C2 . 1.492(7)    yes
C2 . C3 . 1.383(7)    yes
C2 . C5 . 1.393(6)    yes
C3 . C4 . 1.381(7)    yes
C3 . H31 . 0.954    no
C4 . C6 . 1.511(11)    yes
C5 . H51 . 0.937    no
C7 . H71 12_555 1.225    no
C7 . H71 . 0.964    no
C7 . H72 . 0.963    no
C7 . H73 . 0.960    no
C8 . C9 . 1.54(3)    yes
C9 . H92 3_665 0.998    no
C9 . C9 3_665 1.69(2)    yes
C9 . C9 5_565 1.69(2)    yes
C9 . H91 . 0.917    no
C9 . H92 . 0.998    no
H71 . H71 12_555 0.606    no
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
O1 11_665 Cu1 . O2 2_667 89.9(2)    yes
O1 11_665 Cu1 . O2 12_557 168.95(16)    yes
O2 2_667 Cu1 . O2 12_557 89.3(3)    yes
O1 11_665 Cu1 . Cu1 2_667 84.29(12)    yes
O2 2_667 Cu1 . Cu1 2_667 84.67(12)    yes
O2 12_557 Cu1 . Cu1 2_667 84.67(12)    yes
O1 11_665 Cu1 . N1 . 98.8(3)    yes
O2 2_667 Cu1 . N1 . 92.3(3)    yes
O2 12_557 Cu1 . N1 . 92.3(3)    yes
Cu1 2_667 Cu1 . N1 . 175.7(4)    yes
O1 11_665 Cu1 . O1 . 88.7(3)    yes
O2 2_667 Cu1 . O1 . 168.95(16)    yes
O2 12_557 Cu1 . O1 . 89.9(2)    yes
Cu1 2_667 Cu1 . O1 . 84.29(12)    yes
N1 . Cu1 . O1 . 98.8(3)    yes
O1 11_665 Cu1 . O3 . 92.8(2)    yes
O2 2_667 Cu1 . O3 . 98.18(19)    yes
O2 12_557 Cu1 . O3 . 98.18(19)    yes
Cu1 2_667 Cu1 . O3 . 176.0(2)    yes
N1 . Cu1 . O3 . 8.3(6)    yes
O1 . Cu1 . O3 . 92.8(2)    yes
Cu1 . N1 . C8 . 164.3(8)    yes
Cu1 . O1 . C1 . 123.0(3)    yes
Cu1 2_667 O2 . C1 . 123.0(4)    yes
Cu1 . O3 . H101 11_665 103.0    no
Cu1 . O3 . H101 . 103.0    no
H101 11_665 O3 . H101 . 118.6    no
C6 . O4 . C7 . 122.8(10)    yes
O2 . C1 . O1 . 125.1(5)    yes
O2 . C1 . C2 . 117.4(5)    yes
O1 . C1 . C2 . 117.5(4)    yes
C1 . C2 . C3 . 121.2(5)    yes
C1 . C2 . C5 . 119.6(5)    yes
C3 . C2 . C5 . 119.3(5)    yes
C2 . C3 . C4 . 120.7(5)    yes
C2 . C3 . H31 . 119.1    no
C4 . C3 . H31 . 120.2    no
C3 7_655 C4 . C3 . 119.7(7)    yes
C3 7_655 C4 . C6 . 120.1(4)    yes
C3 . C4 . C6 . 120.1(4)    yes
C2 . C5 . C2 7_655 120.2(7)    yes
C2 . C5 . H51 . 119.9    no
C2 7_655 C5 . H51 . 119.9    no
C4 . C6 . O4 . 117.1(4)    yes
C4 . C6 . O4 7_655 117.1(4)    yes
O4 . C6 . O4 7_655 125.7(9)    yes
H71 12_555 C7 . O4 . 133.4    no
H71 12_555 C7 . H71 . 29.1    no
O4 . C7 . H71 . 111.3    no
H71 12_555 C7 . H72 . 106.6    no
O4 . C7 . H72 . 111.3    no
H71 . C7 . H72 . 107.3    no
H71 12_555 C7 . H73 . 80.4    no
O4 . C7 . H73 . 111.6    no
H71 . C7 . H73 . 107.5    no
H72 . C7 . H73 . 107.6    no
N1 . C8 . C9 . 175.4(8)    yes
C8 . C9 . H92 3_665 107.4    no
C8 . C9 . C9 3_665 138.6(3)    yes
H92 3_665 C9 . C9 3_665 31.9    no
C8 . C9 . C9 5_565 138.6(3)    yes
H92 3_665 C9 . C9 5_565 87.5    no
C9 3_665 C9 . C9 5_565 60.000    yes
C8 . C9 . H91 . 111.3    no
H92 3_665 C9 . H91 . 111.6    no
C9 3_665 C9 . H91 . 97.5    no
C9 5_565 C9 . H91 . 97.5    no
C8 . C9 . H92 . 107.4    no
H92 3_665 C9 . H92 . 107.2    no
C9 3_665 C9 . H92 . 87.5    no
C9 5_565 C9 . H92 . 31.9    no
H91 . C9 . H92 . 111.6    no
H71 12_555 H71 . C7 . 100.2    no
H71 12_555 H71 . C7 12_555 50.7    no
C7 . H71 . C7 12_555 132.6    no
C9 5_565 H92 . C9 . 116.2    no
loop_
 _geom_hbond_atom_site_label_D
 _geom_hbond_site_symmetry_D
 _geom_hbond_atom_site_label_H
 _geom_hbond_site_symmetry_H
 _geom_hbond_atom_site_label_A
 _geom_hbond_site_symmetry_A
 _geom_hbond_angle_DHA
 _geom_hbond_distance_DH
 _geom_hbond_distance_HA
 _geom_hbond_distance_DA
 _geom_hbond_publ_flag
C7 . H71 . O4 12_555 136.8(10) 0.964 2.395 3.167(14)    yes
C7 . H71 . C7 12_555 132.6(19) 0.964 1.225 2.007(14)    yes
C9 . H92 . C8 5_565 159.6(7) 0.998 2.073 3.028(14)    yes
C9 5_565 H92 . C8 . 159.6(7) 0.998 2.073 3.028(14)    yes


_iucr_refine_instruction_details_constraints
;
#
# Punched on 30/10/12 at 17:07:52
#
#LIST     12                                                                    
BLOCK 
CONT SCALE 
CONT CU   (    1 ,X'S,U'S) 
CONT N    (    1 ,X'S,U[ISO]) 
CONT O    (    1 ,X'S,U'S)  UNTIL O    (    2 ) 
CONT O    (    3 ,X'S,U[ISO]) 
CONT O    (    4 ,X'S,U'S)  UNTIL C    (    7 ) 
CONT C    (    8 ,X'S,U[ISO])  UNTIL C    (    9 ) 
END                                                                             
;


_iucr_refine_instruction_details_restraints
;
#
# Punched on 30/10/12 at 17:07:52
#
#LIST     16                                                                    
NO 
DISTANCE 1.450000 , 0.050000 = C(9) TO C(8) 
DISTANCE 1.130000 , 0.050000 = N(1) TO C(8) 
DISTANCE 2.180000 , 0.050000 = CU(1) TO N(1) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(73) 
DISTANCE 2.000000 , 0.050000 = CU(1) TO N(1) 
DISTANCE 0.780000 , 0.050000 = O(3) TO H(101) 
ANGLE 180.000000 , 1.000000 = N(1) TO C(8) TO C(9) 
ANGLE 110.000000 , 1.000000 = C(8) TO C(9) TO H(92) 
ANGLE 110.000000 , 1.000000 = C(8) TO C(9) TO H(91) 
ANGLE 170.000000 , 1.000000 = CU(1) TO N(1) TO C(8) 
ANGLE 90.000000 , 1.000000 = N(1) TO CU(1) TO O(1) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00500 = N(1) TO O(1,6,1,1,1) 
VIBR .0, 0.00500 = N(1) TO O(2,-1,1,1,1,2) 
VIBR .0, 0.00500 = N(1) TO O(2,-6,1,0,0,2) 
VIBR .0, 0.00500 = O(3) TO O(1,6,1,1,1) 
VIBR .0, 0.00500 = O(3) TO O(2,-1,1,1,1,2) 
VIBR .0, 0.00500 = O(3) TO O(2,-6,1,0,0,2) 
VIBR .0, 0.00500 = O(3) TO N(1) 
VIBR .0, 0.00500 = O(1) TO N(1) 
VIBR .0, 0.00500 = O(1) TO O(3) 
VIBR .0, 0.00200 = N(1) TO C(8) 
VIBR .0, 0.00200 = C(9) TO C(8) 
VIBR .0, 0.00500 = N(1) TO C(9) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = O(1) TO C(1) 
U(IJ) .0, 0.04000 = C(1) TO O(2) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.04000 = C(2) TO C(5) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(4) TO C(6) 
U(IJ) .0, 0.04000 = C(6) TO O(4,4,1,1) 
U(IJ) .0, 0.04000 = C(6) TO O(4) 
U(IJ) .0, 0.08000 = O(4) TO C(7) 
U(IJ) .0, 0.04000 = N(1) TO C(8) 
U(IJ) .0, 0.08000 = C(9) TO C(8) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
VIBRATION 0.0, 0.020000 = O(4) TO C(7) 
VIBRATION 0.0, 0.020000 = C(6) TO C(7) 
VIBRATION 0.0, 0.020000 = C(4) TO O(4) 
END                                                                             
;

#===END

data_ST1011 
_audit_creation_date        "13-06-10"
_audit_creation_method CRYSTALS_ver_14.40

_oxford_structure_analysis_title  'ST2030 in P-3m1'
_chemical_name_systematic         ?
_chemical_melting_point           ?

#looking for refcif 
 
_publ_contact_author_name         'Scott C. McKellar' 
_publ_contact_author_address 
; 
 Dr Scott C. McKellar 
 The University of Edinburgh 
 Joseph Black Building 
 West Mains Road 
 Edinburgh 
 EH9 3JJ 
; 
 
_publ_contact_author_phone        '+44(0)131 6504804' 
_publ_contact_author_email        'smckella@staffmail.ed.ac.uk' 
 
;

#==============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 

601_ALERT_2_A Structure Contains Solvent Accessible VOIDS of .        219 A**3
041_ALERT_1_C Calc. and Reported SumFormula    Strings  Differ          ?
042_ALERT_1_C Calc. and Reported MoietyFormula Strings  Differ          ?


Structure is a porous framework with disordered solvent in the pores.
The solvent region was treated by the van der Sluis and Spek method, accounting
for 55 e/cell.See below. This corresponds to, within acceptable errors, 
1 molecule of water in the small pore and 0.5 molecules of THF in the large 
pore, per formula unit. F(000), M, mu, D and the given formulae 
have been calculated on this assumption.


027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............      17.70 Deg.
023_ALERT_3_B Resolution (too) Low [sin(theta)/Lambda < 0.6]..      23.30 Deg.


The crystals obtained were small and weakly-diffracting. The biggest crystal
available was selcted and a long exposure time was used to maximise resolution 
and data quality.


201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) .......          1
301_ALERT_3_G Note: Main Residue  Disorder ...................         15 Perc.


There is disordered ligands coordinated to each copper atom which cannot be 
modelled anisotropically.Each coordination site is part-occupied by 
methylamine (one third) and water (two thirds).


045_ALERT_1_C Calculated and Reported Z Differ by ............       0.50 Ratio


This reflects the choice of formula unit


152_ALERT_1_C The Supplied and Calc. Volume s.u. Differ by ...         13 Units

This is due to rounding errors


250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.54

The use of restraints in the refinement mean that off diagonal terms in the
variance-covariance matrix are significant, and the diagonal approximation
used in Platon/Checkcif is subject to error 


303_ALERT_2_C Full Occupancy H-Atom  H101   with # Connections          2

Shared between two part-occupied atoms


341_ALERT_3_C Low Bond Precision on  C-C Bonds (x 1000) Ang ..         12

This is due to the lack of high angle data and disorder of the coordinated 
ligand.



746_ALERT_1_C H...A   Calc     2.44(6), Rep     2.44000 ......    Missing su
              H101 -O1      1.555   2.667                    #         31
746_ALERT_1_C H...A   Calc     2.44(6), Rep     2.44000 ......    Missing su
              H101 -O1      1.555   2.667                    #         31
004_ALERT_5_G Info: Polymeric Structure Found with Dimension .          1
760_ALERT_1_G CIF Contains no Torsion Angles .................          ?
811_ALERT_5_G No ADDSYM Analysis: Too Many Excluded Atoms ....          !

No action taken


910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) .....          1
911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.556         13
909_ALERT_3_G Percentage of Observed Data at Theta(Max) still          38 Perc.
960_ALERT_3_G Number of Intensities with I .LT. - 2*sig(I) ..           1
950_ALERT_5_G Reported and Calculated Hmax Values Differ by ..          3

This is due to weak data at high angle. Data collection was performed as a 
sphere, so was not optimised. Data is still 98.7% complete (see below), 
and data was included to as high an angle as possible in the refinement.

Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged)
Theta sin(th)/Lambda Complete  Expected Measured  Missing
-------------------------------------------------------------------------------
 20.82     0.500     0.994          810      805        5
 23.01     0.550     0.989         1078     1066       12
 23.30     0.556     0.987         1107     1093       14
------------------------------------------------------------ ACTA Min. Res. ---



779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #         48
              H71  -C7   -H71    12.556   1.555   1.555             32.90 Deg.
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #         71
              O3   -H101 -N1      1.555   1.555   1.555             14.00 Deg.

Not a real bond


808_ALERT_5_G No Parseable SHELXL Style Weighting Scheme Found          !

A Shelx weighting scheme was not used.


860_ALERT_3_G Note: Number of Least-Squares Restraints .......         95

Thermal similarity, vibration and distance  restraints required due to 
disordered ligands.


929_ALERT_5_G No Weight Pars,Obs and Calc R1,wR2,S not checked          !


These have been included.
#==============================================================================
;

loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000 -0.009       215        36 ' '
   2  0.333  0.667  0.431        46        10 ' '
   3  0.667  0.333  0.568        46        10 ' '
_platon_squeeze_details
;
see above for details
;


 
_publ_section_exptl_refinement 
; 
; 
 
_publ_section_exptl_prep 
# Brief details or a reference. Include solvent if known 
; 
? 
; 
 
#end of refcif 
_cell_length_a                    18.626(3)
_cell_length_b                    18.626(3)
_cell_length_c                    6.8687(15)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      2063.8(7)
 
_symmetry_cell_setting            'trigonal' 
_symmetry_space_group_name_H-M    'P -3 m 1 ' 
_symmetry_space_group_name_Hall   '-P 3 2' 
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 '-x,-y,-z'
 '-y,x-y,z'
 'y,-x+y,-z'
 '-x+y,-x,z'
 'x-y,x,-z'
 '-x+y,y,z'
 'x-y,-y,-z'
 'x,x-y,z'
 '-x,-x+y,-z'
 '-y,-x,z'
 'y,x,-z'

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source  
 C       0.0033   0.0016   2.3100  20.8439   1.0200  10.2075   1.5886   0.5687
   0.8650  51.6512   0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 H       0.0000   0.0000   0.4930  10.5109   0.3229  26.1257   0.1402   3.1424
   0.0408  57.7998   0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 Cu      0.3201   1.2651  13.3380   3.5828   7.1676   0.2470   5.6158  11.3966
   1.6735  64.8126   1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 N       0.0061   0.0033  12.2126   0.0057   3.1322   9.8933   2.0125  28.9975
   1.1663   0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 O       0.0106   0.0060   3.0485  13.2771   2.2868   5.7011   1.5463   0.3239
   0.8670  32.9089   0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 
 
_cell_formula_units_Z                    2

# Given Formula = C33 H35 Cu3 N1 O21.50 
# Dc =      1.57 Fooo =    937.99 Mu =     16.14 M =    163.04
# Found Formula = C31.00 H29.00 Cu3 N1.00 O20.00 
# Dc =      1.49 FOOO =    937.99 Mu =     16.07 M =    154.37

_chemical_formula_sum             'C33 H35 Cu3 N1 O21.50'
_chemical_formula_moiety          'C33 H35 Cu3 N1 O21.50'
_chemical_compound_source                ?
_chemical_formula_weight            980.26
 
 
_cell_measurement_reflns_used         1870
_cell_measurement_theta_min              2
_cell_measurement_theta_max             23
_cell_measurement_temperature          150
 
_exptl_crystal_description        'plate' 
_exptl_crystal_colour             'blue' 
_exptl_crystal_size_min           0.020 
_exptl_crystal_size_mid           0.030 
_exptl_crystal_size_max           0.050 
 
_exptl_crystal_density_diffrn     1.578 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              998.00 
_exptl_absorpt_coefficient_mu     1.607 
 
# Sheldrick geometric approximatio 0.95 0.97 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'SADABS (Siemens, 1996)' 
_exptl_absorpt_correction_T_min   0.70 
_exptl_absorpt_correction_T_max   0.97 
_diffrn_measurement_device_type   'Bruker Kappa Apex2' 
_diffrn_measurement_device        'Area' 
_diffrn_radiation_monochromator   'graphite' 
_diffrn_radiation_type            'Mo K\a'
_diffrn_radiation_wavelength           0.71073
_diffrn_measurement_method        'φ & ω scans' 
 
# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection        'Apex2 (Bruker AXS, 2006)' 
_computing_cell_refinement        'Apex2 (Bruker AXS, 2006)' 
_computing_data_reduction         'Apex2 (Bruker AXS, 2006)' 
_computing_structure_solution     'SIR92 (Altomare et al., 1994)' 
_computing_structure_refinement   'CRYSTALS (Betteridge et al., 2003)' 
_computing_publication_material   'CRYSTALS (Betteridge et al., 2003)' 
_computing_molecular_graphics     'CAMERON (Watkin et al., 1996)' 
 
_diffrn_standards_interval_time   . 
_diffrn_standards_interval_count  . 
_diffrn_standards_number          0 
_diffrn_standards_decay_%         ? 
 
_diffrn_ambient_temperature        150
_diffrn_reflns_number             6795 
_reflns_number_total              1095 
_diffrn_reflns_av_R_equivalents   0.094 
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 1095 
# Theoretical number of reflections is about 1986 
 
 
_diffrn_reflns_theta_min          2.187 
_diffrn_reflns_theta_max          23.295 
_diffrn_measured_fraction_theta_max 0.989 
 
_diffrn_reflns_theta_full         17.704 
_diffrn_measured_fraction_theta_full 0.995 
 
 
_diffrn_reflns_limit_h_min        -17 
_diffrn_reflns_limit_h_max        0 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        20 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        7 
_reflns_limit_h_min               -17 
_reflns_limit_h_max               0 
_reflns_limit_k_min               0 
_reflns_limit_k_max               20 
_reflns_limit_l_min               0 
_reflns_limit_l_max               7 
 
_oxford_diffrn_Wilson_B_factor    1.63 
_oxford_diffrn_Wilson_scale       121.88 
 
_atom_sites_solution_primary      direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    difmap
 
_refine_diff_density_min          -1.29 
_refine_diff_density_max          1.45 
 
 
# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 
 
 
# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref     I>-10.0\s(I)
_refine_ls_number_reflns          1083 
_refine_ls_number_restraints      95 
_refine_ls_number_parameters      100 
_oxford_refine_ls_R_factor_ref    0.1000 
_refine_ls_wR_factor_ref          0.1534 
_refine_ls_goodness_of_fit_ref    0.9335 
_refine_ls_shift/su_max           0.0008494 
_refine_ls_shift/su_mean          0.0000251 
 
 
# The values computed with all filters except I/sigma 
_oxford_reflns_number_all         1083 
_refine_ls_R_factor_all           0.1000 
_refine_ls_wR_factor_all          0.1534 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0σ(I)
_reflns_number_gt                 736 
_refine_ls_R_factor_gt            0.0619 
_refine_ls_wR_factor_gt           0.1356 
 
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration  '.' 
 
 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full
_refine_ls_hydrogen_treatment     mixed          #undef, noref, refall,
                                                 # refxyz, refU, constr or mixed
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.06P)² +16.03P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
# Insert your own references if required - in alphabetical order 
_publ_section_references 
; 
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., 
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. 
 
Betteridge, P.W., Carruthers, J.R., Cooper, R.I., 
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 
 
Bruker Analytical X-ray Systems, Inc., 2006. Apex2, 
Version 2 User Manual, M86-E01078, Madison, WI. 
 
Siemens Industrial Automation, Inc (1996). 
SADABS: Area-Detector Absorption Correction;: Madison, WI. 
 
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical 
Crystallography Laboratory, Oxford, UK. 
; 

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cu1 Cu 0.52333(4) 0.47667(4) 1.34369(16) 0.0255 1.0000 Uani DS T . . . . 
O1 O 0.5581(3) 0.5895(3) 1.2539(7) 0.0383 1.0000 Uani . U . . . . 
O2 O 0.5194(4) 0.6291(3) 1.5196(7) 0.0459 1.0000 Uani . U . . . . 
O3 O 0.5619(5) 0.4381(5) 1.092(2) 0.038(2) 0.6670 Uiso DS U . . . . 
O4 O 0.7160(4) 0.7986(4) 0.7526(8) 0.0730 1.0000 Uani . U . . . . 
C1 C 0.5504(5) 0.6413(5) 1.3529(10) 0.0329 1.0000 Uani . U . . . . 
C2 C 0.5770(5) 0.7237(4) 1.2653(9) 0.0320 1.0000 Uani . U . . . . 
C3 C 0.6223(5) 0.7472(5) 1.0915(11) 0.0354 1.0000 Uani . U . . . . 
C4 C 0.6464(7) 0.8232(3) 1.0059(14) 0.0356 1.0000 Uani S TU . . . . 
C5 C 0.5565(7) 0.7783(3) 1.3507(14) 0.0338 1.0000 Uani S TU . . . . 
C6 C 0.6972(8) 0.8486(4) 0.8247(18) 0.0528 1.0000 Uani S TU . . . . 
C7 C 0.7609(14) 0.8133(14) 0.577(3) 0.0855 0.5000 Uani . U . . . . 
C8 C 0.6000(9) 0.4000(9) 1.097(5) 0.038(3) 0.3330 Uiso DS U . . . . 
N1 N 0.5557(11) 0.4443(11) 1.073(6) 0.037(3) 0.3330 Uiso DS U . . . . 
H31 H 0.6353 0.7084 1.0268 0.0463 1.0000 Uiso . . . . . . 
H51 H 0.5279 0.7639 1.4719 0.0427 1.0000 Uiso . . . . . . 
H71 H 0.7690 0.7662 0.5483 0.1007 0.5000 Uiso . . . . . . 
H72 H 0.8150 0.8609 0.5868 0.1007 0.5000 Uiso . . . . . . 
H73 H 0.7327 0.8195 0.4699 0.1007 0.5000 Uiso . . . . . . 
H101 H 0.5096(14) 0.4133(13) 1.052(9) 0.0500 1.0000 Uiso D . . . . . 
H81 H 0.6154 0.3846 0.9740 0.0410 0.3330 Uiso . . . . . . 
H82 H 0.6555 0.4278 1.1695 0.0410 0.6670 Uiso . . . . . . 
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0335(6) 0.0335(6) 0.0137(6) 0.0002(3) -0.0002(3) 0.0200(7) 
O1 0.055(4) 0.034(3) 0.028(3) 0.004(2) 0.013(2) 0.023(3) 
O2 0.080(4) 0.040(3) 0.029(3) 0.007(2) 0.016(3) 0.039(3) 
O4 0.109(6) 0.080(5) 0.054(4) 0.020(3) 0.045(4) 0.065(4) 
C1 0.046(5) 0.037(3) 0.024(3) 0.001(2) 0.002(3) 0.026(4) 
C2 0.042(5) 0.033(3) 0.023(3) 0.000(2) -0.002(3) 0.020(4) 
C3 0.043(5) 0.035(4) 0.032(4) 0.001(3) 0.006(3) 0.023(4) 
C4 0.046(7) 0.037(3) 0.027(5) 0.0029(19) 0.006(4) 0.023(4) 
C5 0.048(7) 0.036(3) 0.021(5) 0.000(2) 0.000(4) 0.024(3) 
C6 0.063(8) 0.051(3) 0.048(6) 0.013(2) 0.027(5) 0.032(4) 
C7 0.095(17) 0.108(17) 0.043(10) -0.009(10) 0.029(9) 0.042(13) 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 0.13810(18) 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
Cu1 . O1 11_665 1.963(5)    yes
Cu1 . O2 2_668 1.956(5)    yes
Cu1 . O2 12_558 1.956(5)    yes
Cu1 . Cu1 2_668 2.622(2)    yes
Cu1 . O1 . 1.963(5)    yes
Cu1 . O3 . 2.131(17)    yes
Cu1 . N1 . 2.13(4)    yes
O1 . C1 . 1.247(8)    yes
O2 . C1 . 1.251(8)    yes
O3 . H101 11_665 0.886(10)    no
O3 . H101 . 0.886(10)    no
O4 . C6 . 1.249(7)    yes
O4 . C7 . 1.413(18)    yes
C1 . C2 . 1.484(10)    yes
C2 . C3 . 1.400(10)    yes
C2 . C5 . 1.382(8)    yes
C3 . C4 . 1.384(9)    yes
C3 . H31 . 0.977    no
C4 . C6 . 1.490(15)    yes
C5 . H51 . 0.952    no
C7 . H71 12_556 1.231    no
C7 . H71 . 0.984    no
C7 . H72 . 0.956    no
C7 . H73 . 0.945    no
C8 . H82 11_665 1.025    no
C8 . N1 . 1.44(4)    yes
C8 . H81 . 0.979    no
C8 . H82 . 1.025    no
N1 . H101 11_665 0.77(2)    no
N1 . H101 . 0.77(2)    no
H71 . H71 12_556 0.670    no
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
O1 11_665 Cu1 . O2 2_668 89.4(2)    yes
O1 11_665 Cu1 . O2 12_558 168.2(2)    yes
O2 2_668 Cu1 . O2 12_558 89.9(3)    yes
O1 11_665 Cu1 . Cu1 2_668 83.65(14)    yes
O2 2_668 Cu1 . Cu1 2_668 84.57(15)    yes
O2 12_558 Cu1 . Cu1 2_668 84.57(15)    yes
O1 11_665 Cu1 . O1 . 88.9(3)    yes
O2 2_668 Cu1 . O1 . 168.2(2)    yes
O2 12_558 Cu1 . O1 . 89.4(2)    yes
Cu1 2_668 Cu1 . O1 . 83.65(14)    yes
O1 11_665 Cu1 . O3 . 96.8(3)    yes
O2 2_668 Cu1 . O3 . 95.0(3)    yes
O2 12_558 Cu1 . O3 . 95.0(3)    yes
Cu1 2_668 Cu1 . O3 . 179.3(4)    yes
O1 . Cu1 . O3 . 96.8(3)    yes
O1 11_665 Cu1 . N1 . 92.3(8)    yes
O2 2_668 Cu1 . N1 . 99.5(7)    yes
O2 12_558 Cu1 . N1 . 99.5(7)    yes
Cu1 2_668 Cu1 . N1 . 174.3(11)    yes
O1 . Cu1 . N1 . 92.3(8)    yes
O3 . Cu1 . N1 . 6.4(14)    yes
Cu1 . O1 . C1 . 123.6(4)    yes
Cu1 2_668 O2 . C1 . 122.8(5)    yes
H101 11_665 O3 . Cu1 . 87(5)    no
H101 11_665 O3 . H101 . 108.2(10)    no
Cu1 . O3 . H101 . 87(5)    no
C6 . O4 . C7 . 123.6(12)    yes
O2 . C1 . O1 . 125.4(7)    yes
O2 . C1 . C2 . 116.4(6)    yes
O1 . C1 . C2 . 118.2(6)    yes
C1 . C2 . C3 . 120.4(6)    yes
C1 . C2 . C5 . 121.0(6)    yes
C3 . C2 . C5 . 118.5(7)    yes
C2 . C3 . C4 . 121.2(7)    yes
C2 . C3 . H31 . 119.4    no
C4 . C3 . H31 . 119.4    no
C3 . C4 . C3 9_565 118.8(9)    yes
C3 . C4 . C6 . 120.6(5)    yes
C3 9_565 C4 . C6 . 120.6(5)    yes
C2 . C5 . C2 9_565 121.6(9)    yes
C2 . C5 . H51 . 119.2    no
C2 9_565 C5 . H51 . 119.2    no
C4 . C6 . O4 9_565 117.7(6)    yes
C4 . C6 . O4 . 117.7(6)    yes
O4 9_565 C6 . O4 . 124.6(11)    yes
O4 . C7 . H71 12_556 134.8    no
O4 . C7 . H71 . 109.8    no
H71 12_556 C7 . H71 . 32.9    no
O4 . C7 . H72 . 111.7    no
H71 12_556 C7 . H72 . 105.6    no
H71 . C7 . H72 . 106.2    no
O4 . C7 . H73 . 112.2    no
H71 12_556 C7 . H73 . 76.7    no
H71 . C7 . H73 . 107.1    no
H72 . C7 . H73 . 109.5    no
H82 11_665 C8 . N1 . 119.3    no
H82 11_665 C8 . H81 . 101.4    no
N1 . C8 . H81 . 113.9    no
H82 11_665 C8 . H82 . 98.4    no
N1 . C8 . H82 . 119.3    no
H81 . C8 . H82 . 101.4    no
C8 . N1 . Cu1 . 113(3)    yes
C8 . N1 . H101 11_665 110(4)    no
Cu1 . N1 . H101 11_665 90(7)    no
C8 . N1 . H101 . 110(4)    no
Cu1 . N1 . H101 . 90(7)    no
H101 11_665 N1 . H101 . 137(7)    no
H71 12_556 H71 . C7 . 94.3    no
H71 12_556 H71 . C7 12_556 52.8    no
C7 . H71 . C7 12_556 128.5    no
O3 . H101 . N1 . 14(4)    no
loop_
 _geom_hbond_atom_site_label_D
 _geom_hbond_site_symmetry_D
 _geom_hbond_atom_site_label_H
 _geom_hbond_site_symmetry_H
 _geom_hbond_atom_site_label_A
 _geom_hbond_site_symmetry_A
 _geom_hbond_angle_DHA
 _geom_hbond_distance_DH
 _geom_hbond_distance_HA
 _geom_hbond_distance_DA
 _geom_hbond_publ_flag
C7 . H71 . O4 12_556 132.7(11) 0.984 2.442 3.192(18)    yes
C7 . H71 . C7 12_556 128.5(18) 0.984 1.231 1.998(18)    yes
O3 . H101 . O1 2_667 134(4) 0.886 2.440 3.122(18)    yes
N1 . H101 . O1 2_667 123(6) 0.771 2.440 2.932(18)    yes


_iucr_refine_instruction_details_constraints
;
#
# Punched on 10/06/13 at 16:21:37
#
#LIST     12                                                                    
BLOCK 
CONT SCALE 
CONT CU   (    1 ,X'S,U'S)  UNTIL O    (    2 ) 
CONT O    (    3 ,X'S,U[ISO]) 
CONT O    (    4 ,X'S,U'S)  UNTIL C    (    7 ) 
CONT C    (    8 ,X'S,U[ISO])  UNTIL N    (    1 ) 
CONT H(101, X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints
;
#
# Punched on 10/06/13 at 16:21:37
#
#LIST     16                                                                    
DIST 0.89, 0.01 = O(3) TO H(101) 
ANGLE 108, 1 = H(101) TO O(3) TO H(101, 6, 1, 1, 1) 
DISTANCE 1.400000 , 0.050000 = N(1) TO C(8) 
DISTANCE 2.180000 , 0.050000 = CU(1) TO N(1) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00500 = O(3) TO O(1) 
VIBR .0, 0.00500 = N(1) TO O(1) 
VIBR .0, 0.00500 = N(1) TO O(3) 
VIBR .0, 0.00200 = O(1) TO C(1) 
VIBR .0, 0.00200 = C(1) TO O(2) 
VIBR .0, 0.00200 = C(1) TO C(2) 
VIBR .0, 0.00500 = O(2) TO O(1) 
VIBR .0, 0.00500 = C(2) TO O(1) 
VIBR .0, 0.00500 = C(2) TO O(2) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00200 = C(2) TO C(5) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00500 = C(5) TO C(1) 
VIBR .0, 0.00500 = C(5) TO C(3) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00200 = C(4) TO C(6) 
VIBR .0, 0.00500 = C(6) TO C(3) 
VIBR .0, 0.00500 = C(3) TO C(3,5,1,0,1) 
VIBR .0, 0.00500 = C(6) TO C(3,5,1,0,1) 
VIBR .0, 0.00200 = C(6) TO O(4,5,1,0,1) 
VIBR .0, 0.00200 = C(6) TO O(4) 
VIBR .0, 0.00500 = O(4,5,1,0,1) TO C(4) 
VIBR .0, 0.00500 = O(4) TO C(4) 
VIBR .0, 0.00500 = O(4) TO O(4,5,1,0,1) 
VIBR .0, 0.00200 = O(4) TO C(7) 
VIBR .0, 0.00500 = C(7) TO C(6) 
VIBR .0, 0.00500 = C(2,5,1,0,1) TO C(2) 
VIBR .0, 0.00200 = O(3) TO C(8) 
VIBR .0, 0.00200 = N(1) TO C(8) 
VIBR .0, 0.00500 = O(3) TO N(1) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = O(1) TO C(1) 
U(IJ) .0, 0.04000 = C(1) TO O(2) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(2) TO C(5) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(4) TO C(6) 
U(IJ) .0, 0.04000 = C(6) TO O(4,5,1,0,1) 
U(IJ) .0, 0.04000 = C(6) TO O(4) 
U(IJ) .0, 0.08000 = O(4) TO C(7) 
U(IJ) .0, 0.04000 = O(3) TO C(8) 
U(IJ) .0, 0.04000 = N(1) TO C(8) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
   0   3   1  x   .
  -2   4   1  x   .

#===END

data_ST1012 
_audit_creation_date        "12-11-04"
_audit_creation_method CRYSTALS_ver_14.40

_oxford_structure_analysis_title  'ST2028 in P-3m1'
_chemical_name_systematic         ?
_chemical_melting_point           ?

#looking for refcif 
 
_publ_contact_author_name         'Scott C. McKellar' 
_publ_contact_author_address 
; 
 Dr Scott C. McKellar 
 The University of Edinburgh 
 Joseph Black Building 
 West Mains Road 
 Edinburgh 
 EH9 3JJ 
; 
 
_publ_contact_author_phone        '+44(0)131 6504804' 
_publ_contact_author_email        'smckella@staffmail.ed.ac.uk' 
;

#==============================================================================
>>> The Following Model ALERTS were generated                 - (Acta-Mode) <<<
#==============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
601_ALERT_2_A Structure Contains Solvent Accessible VOIDS of .        216 A**3

Structure is a porous framework with disordered solvent in the pores.
The solvent region was treated by the van der Sluis and Spek method, accounting
for 32 e/cell. See below. This corresponds to, within aceptable errors, 1 
molecule of water in the small pore and 1 molecule of water in the large pore, 
per formula unit. F(000), M, mu, D and the given formulae have been calculated
on this assumption.


201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) .......          1
301_ALERT_3_G Note: Main Residue  Disorder ...................         14 Perc.

There is disordered ligands coordinated to each copper atom which cannot be 
modelled anisotropically.Each coordination site is part-occupied by ethylamine 
(one third) and water (two thirds). 


303_ALERT_2_B Full Occupancy H-Atom  H91    with # Connections          3

Atom is actually part occupied (one third), but is in special position, shared 
between
 ll 3 ligand sites.

303_ALERT_2_B Full Occupancy H-Atom  H101   with # Connections          3

Atom is in the same position for the water and amine hydrogen atoms, therefore
has been set to full occupancy.


023_ALERT_3_C Resolution (too) Low [sin(theta)/Lambda < 0.6]..      24.13 Deg.

The crystals obtained were small and weakly-diffracting. A long exposure time 
was used to maximise resolution and data quality.


152_ALERT_1_C The Supplied and Calc. Volume s.u. Differ by ...         15 Units

This is due to rounding errors.


220_ALERT_2_C Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       3.22 Ratio

This is unsurprising given the coordinated, disorered solvent and disordered 
ester

241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         O1
242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        Cu1

O1 is adjacent to Cu1 which is a heavy atom


341_ALERT_3_C Low Bond Precision on  C-C Bonds (x 1000) Ang ..         12

This is due to the lack of high angle data and disorder of the coordinated 
ligand.


004_ALERT_5_G Info: Polymeric Structure Found with Dimension .          1

Structure is a coordination polymer.


760_ALERT_1_G CIF Contains no Torsion Angles .................          ?

No action taken.

779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #         48
              H71  -C7   -H71    10.556   1.555   1.555             34.90 Deg.
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #         80
              N1   -H101 -O3      1.555   1.555   1.555             13.90 Deg.

Not genuine bonds


808_ALERT_5_G No Parseable SHELXL Style Weighting Scheme Found          !

A Shelx weighting scheme was not used.


811_ALERT_5_G No ADDSYM Analysis: Too Many Excluded Atoms ....          !

No action taken.


860_ALERT_3_G Note: Number of Least-Squares Restraints .......        103

Thermal similarity, vibration, distance and angle restraints required due to 
disordered ligands. 


929_ALERT_5_G No Weight Pars,Obs and Calc R1,wR2,S not checked          !

These have been included.

919_ALERT_3_B Reflection # Likely Affected by the Beamstop ...          1

No action taken


250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.37

The use of restraints in the refinement mean that off diagonal terms in the
variance-covariance matrix are significant, and the diagonal approximation
used in Platon/Checkcif is subject to error 


910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) .....          1
909_ALERT_3_G Percentage of Observed Data at Theta(Max) still          46 Perc.
950_ALERT_5_G Reported and Calculated Hmax Values Differ by ..          3
960_ALERT_3_G Number of Intensities with I .LT. - 2*sig(I) ..           2

This is due to weak data at high angle. Data collection was performed as a 
sphere, so was not optimised. Data is still 99.8% complete (see below), and data 
was included to as high an angle as possible in the refinement.

Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged)
Theta sin(th)/Lambda Complete  Expected Measured  Missing
-------------------------------------------------------------------------------
 20.82     0.500     0.999          800      799        1
 23.01     0.550     0.998         1068     1066        2
 24.13     0.575     0.998         1205     1203        2
------------------------------------------------------------ ACTA Min. Res. ---
#==============================================================================
  
;

loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000 -0.009       212        18 ' '
   2  0.333  0.667  0.482        25         7 ' '
   3  0.667  0.333  0.518        25         7 ' '
_platon_squeeze_details
;
see above for details
;
 
_publ_section_exptl_refinement 
; 
; 
 
_publ_section_exptl_prep 
# Brief details or a reference. Include solvent if known 
; 
? 
; 
 
#end of refcif 
_cell_length_a                    18.577(3)
_cell_length_b                    18.577(3)
_cell_length_c                    6.8410(10)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      2044.5(5)
 
_symmetry_cell_setting            'trigonal' 
_symmetry_space_group_name_H-M    'P -3 m 1 ' 
_symmetry_space_group_name_Hall   '-P 3 2' 
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 '-x,-y,-z'
 '-y,x-y,z'
 'y,-x+y,-z'
 '-x+y,-x,z'
 'x-y,x,-z'
 '-x+y,y,z'
 'x-y,-y,-z'
 'x,x-y,z'
 '-x,-x+y,-z'
 '-y,-x,z'
 'y,x,-z'

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source  
 C       0.0033   0.0016   2.3100  20.8439   1.0200  10.2075   1.5886   0.5687
   0.8650  51.6512   0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 H       0.0000   0.0000   0.4930  10.5109   0.3229  26.1257   0.1402   3.1424
   0.0408  57.7998   0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 O       0.0106   0.0060   3.0485  13.2771   2.2868   5.7011   1.5463   0.3239
   0.8670  32.9089   0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 Cu      0.3201   1.2651  13.3380   3.5828   7.1676   0.2470   5.6158  11.3966
   1.6735  64.8126   1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 N       0.0061   0.0033  12.2126   0.0057   3.1322   9.8933   2.0125  28.9975
   1.1663   0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 
 
_cell_formula_units_Z                    2

# Given Formula = C32.00 H32.00 Cu3 N1 O22 
# Dc =      1.58 Fooo =    949.97 Mu =     16.30 M =    162.21
# Found Formula = C32.00 H29.00 Cu3 N1.00 O20.00 
# Dc =      1.52 FOOO =    949.97 Mu =     16.23 M =    156.36

_chemical_formula_sum             'C32.00 H32.00 Cu3 N1 O22'
_chemical_formula_moiety          'C32.00 H32.00 Cu3 N1 O22'
_chemical_compound_source                ?
_chemical_formula_weight            973.23
 
 
_cell_measurement_reflns_used         2995
_cell_measurement_theta_min              3
_cell_measurement_theta_max             24
_cell_measurement_temperature          150
 
_exptl_crystal_description        'plate' 
_exptl_crystal_colour             'blue' 
_exptl_crystal_size_min           0.030 
_exptl_crystal_size_mid           0.030 
_exptl_crystal_size_max           0.050 
 
_exptl_crystal_density_diffrn     1.581 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              988.00 
_exptl_absorpt_coefficient_mu     1.63 
 
# Sheldrick geometric approximatio 0.95 0.95 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'SADABS (Siemens, 1996)' 
_exptl_absorpt_correction_T_min   0.84 
_exptl_absorpt_correction_T_max   0.95 
_diffrn_measurement_device_type   'Bruker Kappa Apex2' 
_diffrn_measurement_device        'Area' 
_diffrn_radiation_monochromator   'graphite' 
_diffrn_radiation_type            'Mo K\a'
_diffrn_radiation_wavelength           0.71073
_diffrn_measurement_method        'φ & ω scans' 
 
# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection        'Apex2 (Bruker AXS, 2006)' 
_computing_cell_refinement        'Apex2 (Bruker AXS, 2006)' 
_computing_data_reduction         'Apex2 (Bruker AXS, 2006)' 
_computing_structure_solution     'SIR92 (Altomare et al., 1994)' 
_computing_structure_refinement   'CRYSTALS (Betteridge et al., 2003)' 
_computing_publication_material   'CRYSTALS (Betteridge et al., 2003)' 
_computing_molecular_graphics     'CAMERON (Watkin et al., 1996)' 
 
_diffrn_standards_interval_time   . 
_diffrn_standards_interval_count  . 
_diffrn_standards_number          0 
_diffrn_standards_decay_%         ? 
 
_diffrn_ambient_temperature        150
_diffrn_reflns_number             8199 
_reflns_number_total              1203 
_diffrn_reflns_av_R_equivalents   0.059 
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 1203 
# Theoretical number of reflections is about 2173 
 
 
_diffrn_reflns_theta_min          2.193 
_diffrn_reflns_theta_max          24.130 
_diffrn_measured_fraction_theta_max 0.998 
 
_diffrn_reflns_theta_full         24.130 
_diffrn_measured_fraction_theta_full 0.998 
 
 
_diffrn_reflns_limit_h_min        -18 
_diffrn_reflns_limit_h_max        0 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        21 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        7 
_reflns_limit_h_min               -18 
_reflns_limit_h_max               0 
_reflns_limit_k_min               0 
_reflns_limit_k_max               21 
_reflns_limit_l_min               0 
_reflns_limit_l_max               7 
 
_oxford_diffrn_Wilson_B_factor    1.39 
_oxford_diffrn_Wilson_scale       109.25 
 
_atom_sites_solution_primary      direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    difmap
 
_refine_diff_density_min          -1.57 
_refine_diff_density_max          1.92 
 
 
# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 
 
 
# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref     I>-10.0\s(I)
_refine_ls_number_reflns          1193 
_refine_ls_number_restraints      103 
_refine_ls_number_parameters      100 
_oxford_refine_ls_R_factor_ref    0.0863 
_refine_ls_wR_factor_ref          0.1497 
_refine_ls_goodness_of_fit_ref    0.8787 
_refine_ls_shift/su_max           0.0014111 
_refine_ls_shift/su_mean          0.0000372 
 
 
# The values computed with all filters except I/sigma 
_oxford_reflns_number_all         1193 
_refine_ls_R_factor_all           0.0863 
_refine_ls_wR_factor_all          0.1497 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0σ(I)
_reflns_number_gt                 900 
_refine_ls_R_factor_gt            0.0618 
_refine_ls_wR_factor_gt           0.1361 
 
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration  '.' 
 
 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full
_refine_ls_hydrogen_treatment     noref          #undef, noref, refall,
                                                 # refxyz, refU, constr or mixed
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 7.12 8.61 3.45 
;
# Insert your own references if required - in alphabetical order 
_publ_section_references 
; 
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., 
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. 
 
Betteridge, P.W., Carruthers, J.R., Cooper, R.I., 
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 
 
Bruker Analytical X-ray Systems, Inc., 2006. Apex2, 
Version 2 User Manual, M86-E01078, Madison, WI. 
 
Prince, E. 
Mathematical Techniques in Crystallography 
and Materials Science 
Springer-Verlag, New York, 1982. 
 
Siemens Industrial Automation, Inc (1996). 
SADABS: Area-Detector Absorption Correction;: Madison, WI. 
 
Watkin D.J. (1994). 
Acta Cryst, A50, 411-437. 
 
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical 
Crystallography Laboratory, Oxford, UK. 
; 

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cu1 Cu 0.47665(3) 0.52335(3) 1.65643(14) 0.0182 1.0000 Uani DS T . . . . 
O1 O 0.3711(3) 0.4804(3) 1.5197(6) 0.0383 1.0000 Uani D U . . . . 
O2 O 0.4109(3) 0.4416(3) 1.2510(6) 0.0351 1.0000 Uani . U . . . . 
O3 O 0.4401(4) 0.5599(4) 1.9135(19) 0.0361(18) 0.6670 Uiso DS U . . . . 
O4 O 0.0829(4) 0.2858(4) 0.7496(9) 0.0703 1.0000 Uani . U . . . . 
C1 C 0.3598(4) 0.4499(4) 1.3525(9) 0.0226 1.0000 Uani . U . . . . 
C2 C 0.2757(4) 0.4221(4) 1.2599(9) 0.0271 1.0000 Uani . U . . . . 
C3 C 0.2541(4) 0.3782(4) 1.0880(9) 0.0283 1.0000 Uani . U . . . . 
C4 C 0.1771(3) 0.3541(7) 1.0057(15) 0.0358 1.0000 Uani S TU . . . . 
C5 C 0.2221(3) 0.4441(6) 1.3499(13) 0.0252 1.0000 Uani S TU . . . . 
C6 C 0.1523(4) 0.3046(8) 0.8194(17) 0.0479 1.0000 Uani S TU . . . . 
C7 C 0.0509(14) 0.2397(15) 0.582(3) 0.0736 0.5000 Uani . U . . . . 
C8 C 0.3934(8) 0.6066(8) 1.876(3) 0.040(2) 0.3330 Uiso DS U . . . . 
C9 C 0.3655(9) 0.6345(9) 2.050(4) 0.042(3) 0.3330 Uiso DS U . . . . 
N1 N 0.4347(9) 0.5653(9) 1.907(3) 0.038(2) 0.3330 Uiso DS U . . . . 
H31 H 0.2924 0.3650 1.0240 0.0315 1.0000 Uiso . . . . . . 
H51 H 0.2369 0.4737 1.4724 0.0292 1.0000 Uiso . . . . . . 
H71 H -0.0026 0.2327 0.5525 0.0895 0.5000 Uiso . . . . . . 
H72 H 0.0869 0.2679 0.4722 0.0895 0.5000 Uiso . . . . . . 
H73 H 0.0459 0.1864 0.5934 0.0895 0.5000 Uiso . . . . . . 
H81 H 0.3449 0.5716 1.7951 0.0378 0.3330 Uiso . . . . . . 
H91 H 0.3333 0.6667 2.0024 0.0413 1.0000 Uiso . . . . . . 
H92 H 0.3277 0.5888 2.1230 0.0413 0.3330 Uiso . . . . . . 
H101 H 0.4702 0.5778 1.9540 0.0500 1.0000 Uiso D . . . . . 
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0208(5) 0.0208(5) 0.0187(5) 0.0000(2) 0.0000(2) 0.0146(5) 
O1 0.028(2) 0.066(4) 0.031(2) -0.012(2) -0.0044(19) 0.030(3) 
O2 0.029(2) 0.052(3) 0.031(2) -0.014(2) -0.0048(19) 0.026(2) 
O4 0.054(3) 0.097(5) 0.067(4) -0.049(4) -0.034(3) 0.043(4) 
C1 0.025(3) 0.024(3) 0.025(2) 0.003(2) -0.0005(19) 0.016(3) 
C2 0.021(3) 0.030(3) 0.033(3) -0.006(2) -0.002(2) 0.015(3) 
C3 0.022(3) 0.036(4) 0.034(3) -0.007(3) -0.002(2) 0.020(3) 
C4 0.026(3) 0.047(6) 0.042(5) -0.017(4) -0.009(2) 0.023(3) 
C5 0.023(2) 0.031(5) 0.024(4) -0.005(4) -0.0027(18) 0.016(2) 
C6 0.042(3) 0.062(7) 0.047(5) -0.026(5) -0.013(2) 0.031(4) 
C7 0.080(13) 0.099(16) 0.048(9) -0.035(9) -0.029(8) 0.049(13) 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 0.14034(17) 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
Cu1 . O2 2_668 1.957(4)    yes
Cu1 . O2 12_558 1.957(4)    yes
Cu1 . O1 11_665 1.947(5)    yes
Cu1 . Cu1 2_668 2.6150(19)    yes
Cu1 . O1 . 1.947(5)    yes
Cu1 . O3 . 2.116(14)    yes
Cu1 . N1 . 2.18(3)    yes
O1 . C1 . 1.247(7)    yes
O2 . C1 . 1.246(7)    yes
O3 . H101 11_665 0.560    no
O3 . H101 . 0.560    no
O4 . C6 . 1.249(7)    yes
O4 . C7 . 1.378(17)    yes
C1 . C2 . 1.517(8)    yes
C2 . C3 . 1.372(9)    yes
C2 . C5 . 1.396(8)    yes
C3 . C4 . 1.388(8)    yes
C3 . H31 . 0.965    no
C4 . C6 . 1.503(14)    yes
C5 . H51 . 0.964    no
C7 . H71 10_556 1.257    no
C7 . H71 . 0.958    no
C7 . H72 . 0.964    no
C7 . H73 . 0.950    no
C8 . H81 11_665 0.979    no
C8 . C9 . 1.49(3)    yes
C8 . N1 . 1.35(3)    yes
C8 . H81 . 0.979    no
C9 . H92 11_665 0.930    no
C9 . C9 9_565 1.79(5)    yes
C9 . C9 5_565 1.79(5)    yes
C9 . H91 . 1.087    no
C9 . H92 . 0.930    no
N1 . H101 11_665 0.661    no
N1 . H101 . 0.661    no
H71 . H71 10_556 0.724    no
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
O2 2_668 Cu1 . O2 12_558 88.9(3)    yes
O2 2_668 Cu1 . O1 11_665 89.3(2)    yes
O2 12_558 Cu1 . O1 11_665 168.69(18)    yes
O2 2_668 Cu1 . Cu1 2_668 84.22(13)    yes
O2 12_558 Cu1 . Cu1 2_668 84.22(13)    yes
O1 11_665 Cu1 . Cu1 2_668 84.48(13)    yes
O2 2_668 Cu1 . O1 . 168.69(18)    yes
O2 12_558 Cu1 . O1 . 89.3(2)    yes
O1 11_665 Cu1 . O1 . 90.2(3)    yes
Cu1 2_668 Cu1 . O1 . 84.48(13)    yes
O2 2_668 Cu1 . O3 . 94.9(3)    yes
O2 12_558 Cu1 . O3 . 94.9(3)    yes
O1 11_665 Cu1 . O3 . 96.4(3)    yes
Cu1 2_668 Cu1 . O3 . 178.7(3)    yes
O1 . Cu1 . O3 . 96.4(3)    yes
O2 2_668 Cu1 . N1 . 98.0(4)    yes
O2 12_558 Cu1 . N1 . 98.0(4)    yes
O1 11_665 Cu1 . N1 . 93.3(4)    yes
Cu1 2_668 Cu1 . N1 . 176.9(6)    yes
O1 . Cu1 . N1 . 93.3(4)    yes
O3 . Cu1 . N1 . 4.4(8)    yes
Cu1 . O1 . C1 . 122.2(4)    yes
Cu1 2_668 O2 . C1 . 122.1(4)    yes
Cu1 . O3 . H101 11_665 102.5    no
Cu1 . O3 . H101 . 102.5    no
H101 11_665 O3 . H101 . 105.5    no
C6 . O4 . C7 . 123.9(11)    yes
O1 . C1 . O2 . 127.0(6)    yes
O1 . C1 . C2 . 116.6(5)    yes
O2 . C1 . C2 . 116.3(5)    yes
C1 . C2 . C3 . 120.4(6)    yes
C1 . C2 . C5 . 118.8(5)    yes
C3 . C2 . C5 . 120.8(6)    yes
C2 . C3 . C4 . 119.2(6)    yes
C2 . C3 . H31 . 120.4    no
C4 . C3 . H31 . 120.4    no
C3 . C4 . C3 7_555 121.0(9)    yes
C3 . C4 . C6 . 119.5(4)    yes
C3 7_555 C4 . C6 . 119.5(4)    yes
C2 . C5 . C2 7_555 118.9(8)    yes
C2 . C5 . H51 . 120.6    no
C2 7_555 C5 . H51 . 120.6    no
C4 . C6 . O4 7_555 116.9(5)    yes
C4 . C6 . O4 . 116.9(5)    yes
O4 7_555 C6 . O4 . 126.2(10)    yes
O4 . C7 . H71 10_556 136.1    no
O4 . C7 . H71 . 110.7    no
H71 10_556 C7 . H71 . 34.9    no
O4 . C7 . H72 . 110.1    no
H71 10_556 C7 . H72 . 75.4    no
H71 . C7 . H72 . 107.7    no
O4 . C7 . H73 . 111.3    no
H71 10_556 C7 . H73 . 107.5    no
H71 . C7 . H73 . 108.8    no
H72 . C7 . H73 . 108.3    no
H81 11_665 C8 . C9 . 108.8    no
H81 11_665 C8 . N1 . 107.9    no
C9 . C8 . N1 . 117.9(9)    yes
H81 11_665 C8 . H81 . 104.9    no
C9 . C8 . H81 . 108.8    no
N1 . C8 . H81 . 107.9    no
C8 . C9 . H92 11_665 110.2    no
C8 . C9 . C9 9_565 121.4(8)    yes
H92 11_665 C9 . C9 9_565 72.6    no
C8 . C9 . C9 5_565 121.4(8)    yes
H92 11_665 C9 . C9 5_565 122.3    no
C9 9_565 C9 . C9 5_565 60.000(7)    yes
C8 . C9 . H91 . 109.4    no
H92 11_665 C9 . H91 . 106.9    no
C9 9_565 C9 . H91 . 34.3    no
C9 5_565 C9 . H91 . 34.3    no
C8 . C9 . H92 . 110.2    no
H92 11_665 C9 . H92 . 113.1    no
C9 9_565 C9 . H92 . 122.3    no
C9 5_565 C9 . H92 . 72.6    no
H91 . C9 . H92 . 106.9    no
C8 . N1 . Cu1 . 119.1(9)    yes
C8 . N1 . H101 11_665 128.9    no
Cu1 . N1 . H101 11_665 91.9    no
C8 . N1 . H101 . 128.9    no
Cu1 . N1 . H101 . 91.9    no
H101 11_665 N1 . H101 . 84.9    no
H71 10_556 H71 . C7 . 95.8    no
H71 10_556 H71 . C7 10_556 49.3    no
C7 . H71 . C7 10_556 126.5    no
C9 . H91 . C9 5_565 111.3    no
C9 . H91 . C9 3_665 111.3    no
C9 5_565 H91 . C9 3_665 111.3    no
N1 . H101 . O3 . 13.9    no
loop_
 _geom_hbond_atom_site_label_D
 _geom_hbond_site_symmetry_D
 _geom_hbond_atom_site_label_H
 _geom_hbond_site_symmetry_H
 _geom_hbond_atom_site_label_A
 _geom_hbond_site_symmetry_A
 _geom_hbond_angle_DHA
 _geom_hbond_distance_DH
 _geom_hbond_distance_HA
 _geom_hbond_distance_DA
 _geom_hbond_publ_flag
C7 . H71 . O4 10_556 132.9(11) 0.958 2.445 3.175(17)    yes
C7 . H71 . C7 10_556 126.5(18) 0.958 1.257 1.983(17)    yes
C9 . H91 . C8 3_665 123.9(4) 1.087 2.116 2.868(17)    yes
C9 . H91 . C8 5_565 123.9(4) 1.087 2.116 2.868(17)    yes
C9 3_665 H91 . C8 . 123.9(4) 1.087 2.116 2.868(17)    yes
C9 3_665 H91 . C8 5_565 123.9(4) 1.087 2.116 2.868(17)    yes
C9 5_565 H91 . C8 . 123.9(4) 1.087 2.116 2.868(17)    yes
C9 5_565 H91 . C8 3_665 123.9(4) 1.087 2.116 2.868(17)    yes


_iucr_refine_instruction_details_constraints
;
#
# Punched on 04/11/12 at 11:59:23
#
#LIST     12                                                                    
BLOCK 
CONT SCALE 
CONT CU   (    1 ,X'S,U'S)  UNTIL O    (    2 ) 
CONT O    (    3 ,X'S,U[ISO]) 
CONT O    (    4 ,X'S,U'S)  UNTIL C    (    7 ) 
CONT C    (    8 ,X'S,U[ISO])  UNTIL N    (    1 ) 
END                                                                             
;


_iucr_refine_instruction_details_restraints
;
#
# Punched on 04/11/12 at 11:59:23
#
#LIST     16                                                                    
NO 
DISTANCE 1.500000 , 0.050000 = C(8) TO C(9) 
DISTANCE 1.400000 , 0.050000 = N(1) TO C(8) 
DISTANCE 0.900000 , 0.050000 = N(1) TO H(101) 
DISTANCE 0.800000 , 0.050000 = O(3) TO H(101) 
DISTANCE 2.180000 , 0.050000 = CU(1) TO N(1) 
ANGLE 90.000000 , 1.000000 = O(1) TO CU(1) TO O(3) 
ANGLE 118.000000 , 1.000000 = CU(1) TO N(1) TO C(8) 
ANGLE 118.000000 , 1.000000 = N(1) TO C(8) TO C(9) 
ANGLE 90.000000 , 1.000000 = O(1) TO CU(1) TO N(1) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00500 = O(3) TO O(1) 
VIBR .0, 0.00500 = N(1) TO O(1) 
VIBR .0, 0.00500 = N(1) TO O(3) 
VIBR .0, 0.00200 = O(1) TO C(1) 
VIBR .0, 0.00200 = C(1) TO O(2) 
VIBR .0, 0.00200 = C(1) TO C(2) 
VIBR .0, 0.00500 = O(2) TO O(1) 
VIBR .0, 0.00500 = C(2) TO O(1) 
VIBR .0, 0.00500 = C(2) TO O(2) 
VIBR .0, 0.00200 = C(2) TO C(5) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00500 = C(5) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(5) 
VIBR .0, 0.00500 = C(2,4) TO C(2) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00200 = C(4) TO C(6) 
VIBR .0, 0.00500 = C(3) TO C(3,4) 
VIBR .0, 0.00500 = C(6) TO C(3,4) 
VIBR .0, 0.00500 = C(6) TO C(3) 
VIBR .0, 0.00200 = C(6) TO O(4,4) 
VIBR .0, 0.00200 = C(6) TO O(4) 
VIBR .0, 0.00500 = O(4,4) TO C(4) 
VIBR .0, 0.00500 = O(4) TO C(4) 
VIBR .0, 0.00500 = O(4) TO O(4,4) 
VIBR .0, 0.00200 = O(4) TO C(7) 
VIBR .0, 0.00500 = C(7) TO C(6) 
VIBR .0, 0.00200 = O(3) TO C(8) 
VIBR .0, 0.00200 = N(1) TO C(8) 
VIBR .0, 0.00200 = C(8) TO C(9) 
VIBR .0, 0.00500 = N(1) TO O(3) 
VIBR .0, 0.00500 = C(9) TO O(3) 
VIBR .0, 0.00500 = C(9) TO N(1) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = O(1) TO C(1) 
U(IJ) .0, 0.04000 = C(1) TO O(2) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.04000 = C(2) TO C(5) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(4) TO C(6) 
U(IJ) .0, 0.04000 = C(6) TO O(4,4) 
U(IJ) .0, 0.04000 = C(6) TO O(4) 
U(IJ) .0, 0.08000 = O(4) TO C(7) 
U(IJ) .0, 0.04000 = O(3) TO C(8) 
U(IJ) .0, 0.04000 = N(1) TO C(8) 
U(IJ) .0, 0.08000 = C(8) TO C(9) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

#===END

data_ST1013
_audit_creation_date        "13-04-29"
_audit_creation_method CRYSTALS_ver_14.40

_oxford_structure_analysis_title  'ST2039 in P-3m1'
_chemical_name_systematic         ?
_chemical_melting_point           ?

#looking for refcif 
 
_publ_contact_author_name         'Scott C. McKellar' 
_publ_contact_author_address 
; 
 Dr Scott C. McKellar 
 The University of Edinburgh 
 Joseph Black Building 
 West Mains Road 
 Edinburgh 
 EH9 3JJ 
; 
 
_publ_contact_author_phone        '+44(0)131 6504804' 
_publ_contact_author_email        'smckella@staffmail.ed.ac.uk' 
 
_publ_section_exptl_refinement 
;
 
#==============================================================================
>>> The Following Model ALERTS were generated                 - (Acta-Mode) <<<
#==============================================================================
022_ALERT_3_A Ratio Unique / Expected Reflections (too) Low ..       0.73
027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............      17.53 Deg.
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low .......       0.78
023_ALERT_3_B Resolution (too) Low [sin(theta)/Lambda < 0.6]..      23.37 Deg.
341_ALERT_3_B Low Bond Precision on  C-C Bonds (x 1000) Ang ..         17
911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L=  0.558        247
910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) .....          4
913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....         54
088_ALERT_3_C Poor Data / Parameter Ratio ....................       9.36
950_ALERT_5_G Reported and Calculated Hmax Values Differ by ..          5
951_ALERT_5_G Reported and Calculated Kmax Values Differ by ..          2

The high pressure cell causes shading of a significant proportion of the
sphere of reflections. This means that the completeness is reduced and as
such the quality of the model is lower.All of the above are cause by shading 
by the pressure cell.

020_ALERT_3_B The value of Rint is greater than 0.12 .........       0.20

This is caused by weak data and low completeness.


601_ALERT_2_A Structure Contains Solvent Accessible VOIDS of .        244 A**3

Structure is a porous framework with disordered solvent in the pores.
The solvent region was treated by the van der Sluis and Spek method (SQUEEZE), 
accounting for 198 e/cell. See below. This corresponds to 2 molecules of 
acetaldehyde in the large pore and 1 molecules of acetaldehyde in each small 
pore, per formula unit. F(000), M, mu, D and the given formulae have been 
calculated on this assumption.


201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) .......         10

Due to the low number of reflections available, all atoms (except Cu) 
were refined isotropicaly to maximise the data:parameter ratio. 


042_ALERT_1_C Calc. and Reported MoietyFormula Strings  Differ          ?

This is due to the disordered solvent present in the framework pores. 
The solvent was not able to be modelled and thus was handled using 
SQUEEZE. 


045_ALERT_1_C Calculated and Reported Z Differ by ............       3.00 Ratio

This reflects the choice of forumla unit.


152_ALERT_1_C The Supplied and Calc. Volume s.u. Differ by ...          6 Units

This is due to rounding errors.


242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        Cu1

Cu1 is a heavy atom 


303_ALERT_2_C Full Occupancy H-Atom  H71    with # Connections          2

H71 is shared between two 50:50 disordered C atoms, hence is fully occupied.


004_ALERT_5_G Info: Polymeric Structure Found with Dimension .          1
760_ALERT_1_G CIF Contains no Torsion Angles .................          ?

No action taken


301_ALERT_3_G Note: Main Residue  Disorder ...................          5 Perc.

Ester groups are disordered over two sites.


808_ALERT_5_G No Parseable SHELXL Style Weighting Scheme Found          !

A Shelx weighting scheme was not used.


860_ALERT_3_G Note: Number of Least-Squares Restraints .......         53

Thermal similarity, vibration, distance and angle restraints required 
due to disorder and low completeness. 


929_ALERT_5_G No Weight Pars,Obs and Calc R1,wR2,S not checked          !

These have been included
#==============================================================================

; 


loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000 -0.004       224        98 ' '
   2  0.333  0.667  0.003       132        50 ' '
   3  0.667  0.333 -0.050       132        50 ' '
_platon_squeeze_details
;
See above for details.
; 

 
_publ_section_exptl_prep 
# Brief details or a reference. Include solvent if known 
; 
? 
; 
 
#end of refcif 
_cell_length_a                    18.5420(12)
_cell_length_b                    18.5420(12)
_cell_length_c                    6.8114(5)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      2028.1(2)
 
_symmetry_cell_setting            'trigonal' 
_symmetry_space_group_name_H-M    'P -3 m 1 ' 
_symmetry_space_group_name_Hall   '-P 3 2' 
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 '-x,-y,-z'
 '-y,x-y,z'
 'y,-x+y,-z'
 '-x+y,-x,z'
 'x-y,x,-z'
 '-x+y,y,z'
 'x-y,-y,-z'
 'x,x-y,z'
 '-x,-x+y,-z'
 '-y,-x,z'
 'y,x,-z'

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source  
 C       0.0033   0.0016   2.3100  20.8439   1.0200  10.2075   1.5886   0.5687
   0.8650  51.6512   0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 H       0.0000   0.0000   0.4930  10.5109   0.3229  26.1257   0.1402   3.1424
   0.0408  57.7998   0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 O       0.0106   0.0060   3.0485  13.2771   2.2868   5.7011   1.5463   0.3239
   0.8670  32.9089   0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 Cu      0.3201   1.2651  13.3380   3.5828   7.1676   0.2470   5.6158  11.3966
   1.6735  64.8126   1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 
 
_cell_formula_units_Z                    2

# Given Formula = C38.00 H40 Cu3 O25 
# Dc =      1.78 Fooo =    906.00 Mu =     16.58 M =    181.23
# Found Formula = C30 H18 Cu3 O21 
# Dc =      1.48 FOOO =    906.00 Mu =     16.35 M =    150.85

_chemical_formula_sum             'C38.00 H40 Cu3 O25'
_chemical_formula_moiety          'C30 H24 Cu3 O21 .4(CH3CHO)'
_chemical_compound_source                ?
_chemical_formula_weight            1087.34
 
 
_cell_measurement_reflns_used         1291
_cell_measurement_theta_min              3
_cell_measurement_theta_max             22
_cell_measurement_temperature          300
 
_exptl_crystal_description        'rod' 
_exptl_crystal_colour             'blue' 
_exptl_crystal_size_min           0.030 
_exptl_crystal_size_mid           0.040 
_exptl_crystal_size_max           0.100 
 
_exptl_crystal_density_diffrn     1.781 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              1110.00 
_exptl_absorpt_coefficient_mu     1.66 
 
# Sheldrick geometric approximatio 0.94 0.95 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'SADABS (Siemens, 1996)' 
_exptl_absorpt_correction_T_min   0.64 
_exptl_absorpt_correction_T_max   0.95 
_diffrn_measurement_device_type   'Bruker Kappa Apex2' 
_diffrn_measurement_device        'Area' 
_diffrn_radiation_monochromator   'graphite' 
_diffrn_radiation_type            'Mo K\a'
_diffrn_radiation_wavelength           0.71073
_diffrn_measurement_method        ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection        'Apex2 (Bruker AXS, 2006)' 
_computing_cell_refinement        'Apex2 (Bruker AXS, 2006)' 
_computing_data_reduction         'Apex2 (Bruker AXS, 2006)' 
_computing_structure_solution     'SIR92 (Altomare et al., 1994)' 
_computing_structure_refinement   'CRYSTALS (Betteridge et al., 2003)' 
_computing_publication_material   'CRYSTALS (Betteridge et al., 2003)' 
_computing_molecular_graphics     'CAMERON (Watkin et al., 1996)' 
 
_diffrn_standards_interval_time   . 
_diffrn_standards_interval_count  . 
_diffrn_standards_number          0 
_diffrn_standards_decay_%         ? 
 
_diffrn_ambient_temperature        300
_diffrn_ambient_pressure     	  0.7 #GPa
_diffrn_reflns_number             7350 
_reflns_number_total              803 
_diffrn_reflns_av_R_equivalents   0.196 
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 803 
# Theoretical number of reflections is about 1938 
 
 
_diffrn_reflns_theta_min          3.249 
_diffrn_reflns_theta_max          23.372 
_diffrn_measured_fraction_theta_max 0.730 
 
_diffrn_reflns_theta_full         17.529 
_diffrn_measured_fraction_theta_full 0.781 
 
 
_diffrn_reflns_limit_h_min        -15 
_diffrn_reflns_limit_h_max        0 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        18 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        7 
_reflns_limit_h_min               -15 
_reflns_limit_h_max               0 
_reflns_limit_k_min               0 
_reflns_limit_k_max               18 
_reflns_limit_l_min               0 
_reflns_limit_l_max               7 
 
_oxford_diffrn_Wilson_B_factor    2.01 
_oxford_diffrn_Wilson_scale       65.34 
 
_atom_sites_solution_primary      direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    difmap
 
_refine_diff_density_min          -0.93 
_refine_diff_density_max          0.74 
 
 
# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 
 
 
# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref     I>2.0\s(I)
_refine_ls_number_reflns          440 
_refine_ls_number_restraints      53 
_refine_ls_number_parameters      47 
_oxford_refine_ls_R_factor_ref    0.0939 
_refine_ls_wR_factor_ref          0.1018 
_refine_ls_goodness_of_fit_ref    1.0948 
_refine_ls_shift/su_max           0.0005826 
_refine_ls_shift/su_mean          0.0000638 
 
 
# The values computed with all filters except I/sigma 
_oxford_reflns_number_all         797 
_refine_ls_R_factor_all           0.1840 
_refine_ls_wR_factor_all          0.1799 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0σ(I)
_reflns_number_gt                 440 
_refine_ls_R_factor_gt            0.0939 
_refine_ls_wR_factor_gt           0.1018 
 
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration  '.' 
 
 
_refine_ls_structure_factor_coef  F 
_refine_ls_matrix_type            full
_refine_ls_hydrogen_treatment     noref          #undef, noref, refall,
                                                 # refxyz, refU, constr or mixed
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.936 0.231 0.432 
;
# Insert your own references if required - in alphabetical order 
_publ_section_references 
; 
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., 
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. 
 
Betteridge, P.W., Carruthers, J.R., Cooper, R.I., 
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 
 
Bruker Analytical X-ray Systems, Inc., 2006. Apex2, 
Version 2 User Manual, M86-E01078, Madison, WI. 
 
Prince, E. 
Mathematical Techniques in Crystallography 
and Materials Science 
Springer-Verlag, New York, 1982. 
 
Siemens Industrial Automation, Inc (1996). 
SADABS: Area-Detector Absorption Correction;: Madison, WI. 
 
Watkin D.J. (1994). 
Acta Cryst, A50, 411-437. 
 
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical 
Crystallography Laboratory, Oxford, UK. 
; 

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cu1 Cu 0.47635(9) 0.52365(9) 0.1560(3) 0.0263 1.0000 Uani DS T . . . . 
O1 O 0.4404(7) 0.4104(7) 0.2493(12) 0.045(2) 1.0000 Uiso D U . . . . 
O2 O 0.4816(7) 0.3720(7) -0.0172(14) 0.046(2) 1.0000 Uiso D U . . . . 
O3 O 0.4387(5) 0.5613(5) 0.4178(19) 0.050(5) 1.0000 Uiso DS . . . . . 
O4 O 0.2924(6) 0.0860(7) 0.7717(14) 0.058(2) 1.0000 Uiso D U . . . . 
C1 C 0.4502(6) 0.3585(8) 0.1518(16) 0.0460(19) 1.0000 Uiso D U . . . . 
C2 C 0.4239(6) 0.2761(8) 0.2438(15) 0.0464(19) 1.0000 Uiso D U . . . . 
C3 C 0.3823(7) 0.2554(9) 0.4240(18) 0.048(2) 1.0000 Uiso D U . . . . 
C4 C 0.3582(7) 0.1791(4) 0.510(2) 0.051(2) 1.0000 Uiso DS U . . . . 
C5 C 0.4420(7) 0.2210(4) 0.153(2) 0.046(2) 1.0000 Uiso DS U . . . . 
C6 C 0.3130(7) 0.1565(4) 0.698(2) 0.054(2) 1.0000 Uiso DS U . . . . 
C7 C 0.2488(9) 0.0563(13) 0.951(3) 0.058(3) 0.5000 Uiso D U . . . . 
H31 H 0.3781 0.2971 0.4982 0.0596 1.0000 Uiso . . . . . . 
H51 H 0.4698 0.2349 0.0328 0.0579 1.0000 Uiso . . . . . . 
H71 H 0.2382 0.0000 1.0000 0.0660 1.0000 Uiso D . . . . . 
H72 H 0.2790 0.0918 1.0610 0.0660 0.5000 Uiso D . . . . . 
H73 H 0.1951 0.0528 0.9486 0.0660 0.5000 Uiso D . . . . . 
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0235(15) 0.0235(15) 0.0356(13) 0.0002(6) -0.0002(6) 0.0145(17) 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 0.1423(14) 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
Cu1 . O1 11_665 1.965(11)    yes
Cu1 . O2 2_665 1.933(11)    yes
Cu1 . O2 12_555 1.933(11)    yes
Cu1 . Cu1 2_665 2.612(5)    yes
Cu1 . O1 . 1.965(11)    yes
Cu1 . O3 . 2.154(15)    yes
O1 . C1 . 1.253(15)    yes
O2 . C1 . 1.257(15)    yes
O4 . C6 . 1.268(13)    yes
O4 . C7 . 1.42(3)    yes
C1 . C2 . 1.490(16)    yes
C2 . C3 . 1.398(17)    yes
C2 . C5 . 1.373(15)    yes
C3 . C4 . 1.382(17)    yes
C3 . H31 . 0.959    no
C4 . C6 . 1.47(2)    yes
C5 . H51 . 0.931    no
C7 . H71 . 1.017    no
C7 . H72 . 0.968    no
C7 . H73 . 0.966    no
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
O1 11_665 Cu1 . O2 2_665 89.5(5)    yes
O1 11_665 Cu1 . O2 12_555 168.4(4)    yes
O2 2_665 Cu1 . O2 12_555 89.2(7)    yes
O1 11_665 Cu1 . Cu1 2_665 84.0(3)    yes
O2 2_665 Cu1 . Cu1 2_665 84.4(3)    yes
O2 12_555 Cu1 . Cu1 2_665 84.4(3)    yes
O1 11_665 Cu1 . O1 . 89.5(6)    yes
O2 2_665 Cu1 . O1 . 168.4(4)    yes
O2 12_555 Cu1 . O1 . 89.5(5)    yes
Cu1 2_665 Cu1 . O1 . 84.0(3)    yes
O1 11_665 Cu1 . O3 . 95.0(4)    yes
O2 2_665 Cu1 . O3 . 96.6(4)    yes
O2 12_555 Cu1 . O3 . 96.6(4)    yes
Cu1 2_665 Cu1 . O3 . 178.5(4)    yes
O1 . Cu1 . O3 . 95.0(4)    yes
Cu1 . O1 . C1 . 123.1(7)    yes
Cu1 2_665 O2 . C1 . 124.2(8)    yes
C6 . O4 . C7 . 124.3(8)    yes
O2 . C1 . O1 . 124.3(10)    yes
O2 . C1 . C2 . 118.0(8)    yes
O1 . C1 . C2 . 117.7(9)    yes
C1 . C2 . C3 . 120.3(8)    yes
C1 . C2 . C5 . 119.8(7)    yes
C3 . C2 . C5 . 119.9(7)    yes
C2 . C3 . C4 . 120.3(7)    yes
C2 . C3 . H31 . 119.8    no
C4 . C3 . H31 . 119.2    no
C3 . C4 . C3 9_555 119.1(11)    yes
C3 . C4 . C6 . 120.4(6)    yes
C3 9_555 C4 . C6 . 120.4(6)    yes
C2 9_555 C5 . C2 . 120.2(11)    yes
C2 9_555 C5 . H51 . 119.9    no
C2 . C5 . H51 . 119.9    no
C4 . C6 . O4 . 118.3(6)    yes
C4 . C6 . O4 9_555 118.3(6)    yes
O4 . C6 . O4 9_555 123.2(13)    yes
O4 . C7 . H71 . 117.5    no
O4 . C7 . H72 . 112.3    no
H71 . C7 . H72 . 101.2    no
O4 . C7 . H73 . 112.2    no
H71 . C7 . H73 . 105.8    no
H72 . C7 . H73 . 106.7    no
C7 8_557 H71 . C7 . 142.8    no
loop_
 _geom_hbond_atom_site_label_D
 _geom_hbond_site_symmetry_D
 _geom_hbond_atom_site_label_H
 _geom_hbond_site_symmetry_H
 _geom_hbond_atom_site_label_A
 _geom_hbond_site_symmetry_A
 _geom_hbond_angle_DHA
 _geom_hbond_distance_DH
 _geom_hbond_distance_HA
 _geom_hbond_distance_DA
 _geom_hbond_publ_flag
C7 . H71 . O4 8_557 149.6(14) 1.017 2.090 3.012(19)    yes
C7 8_557 H71 . O4 . 149.6(14) 1.017 2.090 3.012(19)    yes
C7 . H71 . C7 8_557 142.8(19) 1.017 1.017 1.927(19)    yes


_iucr_refine_instruction_details_constraints
;
#
# Punched on 29/04/13 at 11:32:10
#
#LIST     12                                                                    
BLOCK 
CONT SCALE 
CONT CU   (    1 ,X'S,U'S) 
CONT O    (    1 ,X'S,U[ISO])  UNTIL C    (    7 ) 
END                                                                             
;


_iucr_refine_instruction_details_restraints
;
#
# Punched on 29/04/13 at 11:32:10
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = O(1) TO C(1) 
VIBR .0, 0.00200 = O(2) TO C(1) 
VIBR .0, 0.00200 = C(1) TO C(2) 
VIBR .0, 0.00500 = O(1) TO O(2) 
VIBR .0, 0.00500 = C(2) TO O(2) 
VIBR .0, 0.00500 = C(2) TO O(1) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00200 = C(2) TO C(5) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00500 = C(5) TO C(1) 
VIBR .0, 0.00500 = C(5) TO C(3) 
VIBR .0, 0.00200 = O(4) TO C(6) 
VIBR .0, 0.00200 = O(4) TO C(7) 
VIBR .0, 0.00500 = C(7) TO C(6) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00200 = C(6) TO C(4) 
VIBR .0, 0.00500 = O(4) TO O(4,5,1,0,1) 
VIBR .0, 0.00500 = C(4) TO O(4,5,1,0,1) 
VIBR .0, 0.00500 = C(4) TO O(4) 
VIBR .0, 0.00500 = C(2,5,1,0,1) TO C(2) 
VIBR .0, 0.00500 = C(3) TO C(6) 
VIBR .0, 0.00500 = C(3,5,1,0,1) TO C(6) 
VIBR .0, 0.00500 = C(3,5,1,0,1) TO C(3) 
VIBR .0, 0.00200 = C(7) TO C(7,-4,1,1,2,-1) 
VIBR .0, 0.00500 = O(4) TO C(7,-4,1,1,2,-1) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.08000 = O(1) TO C(1) 
U(IJ) .0, 0.08000 = O(2) TO C(1) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(2) TO C(5) 
U(IJ) .0, 0.04000 = O(4) TO C(6) 
U(IJ) .0, 0.04000 = O(4) TO C(7) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(6) TO C(4) 
U(IJ) .0, 0.04000 = C(7) TO C(7,-4,1,1,2,-1) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
DISTANCE 2.150000 , 0.050000 = CU(1) TO O(3) 
DISTANCE 1.950000 , 0.050000 = CU(1) TO O(1) 
DISTANCE 1.250000 , 0.050000 = O(1) TO C(1) 
DISTANCE 1.250000 , 0.050000 = C(1) TO O(2) 
DISTANCE 1.490000 , 0.050000 = C(1) TO C(2) 
DISTANCE 1.400000 , 0.050000 = C(2) TO C(5) 
DISTANCE 1.400000 , 0.050000 = C(2) TO C(3) 
DISTANCE 1.400000 , 0.050000 = C(3) TO C(4) 
DISTANCE 1.510000 , 0.050000 = C(4) TO C(6) 
DISTANCE 1.260000 , 0.050000 = C(6) TO O(4) 
DISTANCE 1.430000 , 0.050000 = O(4) TO C(7) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(71) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(72) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(73) 
ANGLE 94.800000 , 1.000000 = O(3) TO CU(1) TO O(1) 
ANGLE 123.000000 , 1.000000 = CU(1) TO O(1) TO C(1) 
ANGLE 120.000000 , 1.000000 = C(1) TO C(2) TO C(5) 
ANGLE 120.000000 , 1.000000 = C(5) TO C(2) TO C(3) 
ANGLE 120.000000 , 1.000000 = C(2) TO C(3) TO C(4) 
ANGLE 120.000000 , 1.000000 = C(3) TO C(4) TO C(6) 
ANGLE 118.000000 , 1.000000 = C(4) TO C(6) TO O(4) 
ANGLE 124.000000 , 1.000000 = C(6) TO O(4) TO C(7) 
ANGLE 118.000000 , 1.000000 = O(2) TO C(1) TO C(2) 
PLANAR 0.010000  C(1) C(2) C(5) C(3) C(4) C(6) O(4) C(7) 
END                                                                             
;


#===END

data_ST1014
_audit_creation_date        "13-04-29"
_audit_creation_method CRYSTALS_ver_14.40

_oxford_structure_analysis_title  'ST2040 in P-3m1'
_chemical_name_systematic         ?
_chemical_melting_point           ?

#looking for refcif 
 
_publ_contact_author_name         'Scott C. McKellar' 
_publ_contact_author_address 
; 
 Dr Scott C. McKellar 
 The University of Edinburgh 
 Joseph Black Building 
 West Mains Road 
 Edinburgh 
 EH9 3JJ 
; 
 
_publ_contact_author_phone        '+44(0)131 6504804' 
_publ_contact_author_email        'smckella@staffmail.ed.ac.uk' 


_publ_section_exptl_refinement 
; 

#==============================================================================
>>> The Following Model ALERTS were generated                 - (Acta-Mode) <<<
#==============================================================================
    
 
023_ALERT_3_A Resolution (too) Low [sin(theta)/Lambda < 0.6]..      19.76 Deg.
027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............      14.82 Deg.
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low .......       0.90
022_ALERT_3_B Ratio Unique / Expected Reflections (too) Low ..       0.86
088_ALERT_3_B Poor Data / Parameter Ratio ....................       7.09
341_ALERT_3_B Low Bond Precision on  C-C Bonds (x 1000) Ang ..         22
911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L=  0.476         89
910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) .....          4
913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....         26
909_ALERT_3_G Percentage of Observed Data at Theta(Max) still          33 Perc.
950_ALERT_5_G Reported and Calculated Hmax Values Differ by ..          3
918_ALERT_3_C Reflection(s) # with I(obs) much smaller I(calc)          1

The high pressure cell causes shading of a significant proportion of the
sphere of reflections. This means that the completeness is reduced and as
such the quality of the model is lower.All of the above are cause by shading 
by the pressure cell.

020_ALERT_3_C The value of Rint is greater than 0.12 .........       0.18
082_ALERT_2_C High R1 Value ..................................       0.11
960_ALERT_3_G Number of Intensities with I .LT. - 2*sig(I) ..           3

These are caused by weak data and low completeness


601_ALERT_2_A Structure Contains Solvent Accessible VOIDS of .        234 A**3

Structure is a porous framework with disordered solvent in the pores.
The solvent region was treated by the van der Sluis and Spek method (SQUEEZE), 
accountingfor 276 e/cell. This corresponds to 3 molecules of acetaldehyde  
in the large pore and 1.5 molecules of acetaldehyde in each small pore, per 
formula unit. F(000), M, mu, D and the given formulae have been calculated 
on this assumption.
               

201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) .......         10

Due to the low number of reflections available, all atoms (except Cu) were 
refined isotropicaly to maximise the data:parameter ratio. 


042_ALERT_1_C Calc. and Reported MoietyFormula Strings  Differ          ?

This is due to the disordered solvent present in the framework pores. The 
solvent was not able to be modelled and thus was handled using SQUEEZE 
as outlined above. 


045_ALERT_1_C Calculated and Reported Z Differ by ............       3.00 Ratio

This reflects the choice of forumla unit.


152_ALERT_1_C The Supplied and Calc. Volume s.u. Differ by ...          8 Units

This is due to rounding errors.


241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         O1
242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        Cu1

Cu1 is a heavy atom refined anisotropically. O1 is bonded to Cu1.


303_ALERT_2_C Full Occupancy H-Atom  H71    with # Connections          2

H71 is shared between two 50:50 disordered C atoms, hence is fully occupied.


004_ALERT_5_G Info: Polymeric Structure Found with Dimension .          1
760_ALERT_1_G CIF Contains no Torsion Angles .................          ?

No action taken.


732_ALERT_1_C Angle   Calc   119.8(16), Rep    119.9(7) ......       2.29 su-Ra
              C2   -C3   -C4      1.555   1.555   1.555      #         25
732_ALERT_1_C Angle   Calc   120.1(13), Rep    120.2(6) ......       2.17 su-Ra
              C3   -C4   -C6      1.555   1.555   1.555      #         29

The use of restraints in the refinement mean that off diagonal terms in the
variance-covariance matrix are significant, and the diagonal approximation
used in Platon/Checkcif is badly in error.


301_ALERT_3_G Note: Main Residue  Disorder ...................          5 Perc.

Ester groups are disordered over two sites.


808_ALERT_5_G No Parseable SHELXL Style Weighting Scheme Found          !

A Shelx weighting scheme was not used.


860_ALERT_3_G Note: Number of Least-Squares Restraints .......         53

Thermal similarity, vibration, distance and angle restraints required due to 
disorder and low completeness. 


929_ALERT_5_G No Weight Pars,Obs and Calc R1,wR2,S not checked          !

These have been included
#============================================================================== 

;

loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000 -0.066       236       144 ' '
   2  0.333  0.667 -0.008       116        66 ' '
   3  0.667  0.333 -0.051       116        66 ' '
_platon_squeeze_details         
;
see above for details 
; 
 
_publ_section_exptl_prep 
# Brief details or a reference. Include solvent if known 
; 
? 
; 
 
#end of refcif 
_cell_length_a                    18.2591(16)
_cell_length_b                    18.2591(16)
_cell_length_c                    6.6274(6)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      1913.5(3)
 
_symmetry_cell_setting            'trigonal' 
_symmetry_space_group_name_H-M    'P -3 m 1 ' 
_symmetry_space_group_name_Hall   '-P 3 2' 
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 '-x,-y,-z'
 '-y,x-y,z'
 'y,-x+y,-z'
 '-x+y,-x,z'
 'x-y,x,-z'
 '-x+y,y,z'
 'x-y,-y,-z'
 'x,x-y,z'
 '-x,-x+y,-z'
 '-y,-x,z'
 'y,x,-z'

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source  
 C       0.0033   0.0016   2.3100  20.8439   1.0200  10.2075   1.5886   0.5687
   0.8650  51.6512   0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 H       0.0000   0.0000   0.4930  10.5109   0.3229  26.1257   0.1402   3.1424
   0.0408  57.7998   0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 O       0.0106   0.0060   3.0485  13.2771   2.2868   5.7011   1.5463   0.3239
   0.8670  32.9089   0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 Cu      0.3201   1.2651  13.3380   3.5828   7.1676   0.2470   5.6158  11.3966
   1.6735  64.8126   1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 
 
_cell_formula_units_Z                    2

# Given Formula = C42 H48 Cu3 O27 
# Dc =      2.04 Fooo =    906.00 Mu =     17.70 M =    195.91
# Found Formula = C30 H18 Cu3 O21 
# Dc =      1.57 FOOO =    906.00 Mu =     17.33 M =    150.85

_chemical_formula_sum             'C42 H48 Cu3 O27'
_chemical_formula_moiety          'C30 H24 Cu3 O21 .6(CH3CHO)'
_chemical_compound_source                ?
_chemical_formula_weight            1175.45
 
 
_cell_measurement_reflns_used          905
_cell_measurement_theta_min              3
_cell_measurement_theta_max             19
_cell_measurement_temperature          300
 
_exptl_crystal_description        'rod' 
_exptl_crystal_colour             'blue' 
_exptl_crystal_size_min           0.030 
_exptl_crystal_size_mid           0.040 
_exptl_crystal_size_max           0.100 
 
_exptl_crystal_density_diffrn     1.875 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              1206.00 
_exptl_absorpt_coefficient_mu     1.633 
 
# Sheldrick geometric approximatio 0.93 0.95 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'SADABS (Siemens, 1996)' 
_exptl_absorpt_correction_T_min   0.61 
_exptl_absorpt_correction_T_max   0.95 
_diffrn_measurement_device_type   'Bruker Kappa Apex2' 
_diffrn_measurement_device        'Area' 
_diffrn_radiation_monochromator   'graphite' 
_diffrn_radiation_type            'Mo K\a'
_diffrn_radiation_wavelength           0.71073
_diffrn_measurement_method        ω/2θ 
 
# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection        'Apex2 (Bruker AXS, 2006)' 
_computing_cell_refinement        'Apex2 (Bruker AXS, 2006)' 
_computing_data_reduction         'Apex2 (Bruker AXS, 2006)' 
_computing_structure_solution     'SIR92 (Altomare et al., 1994)' 
_computing_structure_refinement   'CRYSTALS (Betteridge et al., 2003)' 
_computing_publication_material   'CRYSTALS (Betteridge et al., 2003)' 
_computing_molecular_graphics     'CAMERON (Watkin et al., 1996)' 
 
_diffrn_standards_interval_time   . 
_diffrn_standards_interval_count  . 
_diffrn_standards_number          0 
_diffrn_standards_decay_%         ? 
 
_diffrn_ambient_temperature        300
_diffrn_ambient_pressure    	  0.2 #GPa
_diffrn_reflns_number             6204 
_reflns_number_total              568 
_diffrn_reflns_av_R_equivalents   0.176 
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 568 
# Theoretical number of reflections is about 1150 
 
 
_diffrn_reflns_theta_min          3.333 
_diffrn_reflns_theta_max          19.760 
_diffrn_measured_fraction_theta_max 0.852 
 
_diffrn_reflns_theta_full         14.820 
_diffrn_measured_fraction_theta_full 0.900 
 
 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        0 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        6 
_reflns_limit_h_min               -14 
_reflns_limit_h_max               0 
_reflns_limit_k_min               0 
_reflns_limit_k_max               16 
_reflns_limit_l_min               0 
_reflns_limit_l_max               6 
 
_oxford_diffrn_Wilson_B_factor    2.01 
_oxford_diffrn_Wilson_scale       65.34 
 
_atom_sites_solution_primary      direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    difmap
 
_refine_diff_density_min          -0.71 
_refine_diff_density_max          0.69 
 
 
# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 
 
 
# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref     I>2.0\s(I)
_refine_ls_number_reflns          333 
_refine_ls_number_restraints      53 
_refine_ls_number_parameters      47 
_oxford_refine_ls_R_factor_ref    0.1102 
_refine_ls_wR_factor_ref          0.1332 
_refine_ls_goodness_of_fit_ref    1.1122 
_refine_ls_shift/su_max           0.0003853 
_refine_ls_shift/su_mean          0.0000377 
 
 
# The values computed with all filters except I/sigma 
_oxford_reflns_number_all         560 
_refine_ls_R_factor_all           0.1949 
_refine_ls_wR_factor_all          0.2535 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0σ(I)
_reflns_number_gt                 333 
_refine_ls_R_factor_gt            0.1102 
_refine_ls_wR_factor_gt           0.1332 
 
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration  '.' 
 
 
_refine_ls_structure_factor_coef  F 
_refine_ls_matrix_type            full
_refine_ls_hydrogen_treatment     noref          #undef, noref, refall,
                                                 # refxyz, refU, constr or mixed
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 1.52 0.745 0.932 
;
# Insert your own references if required - in alphabetical order 
_publ_section_references 
; 
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., 
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. 
 
Betteridge, P.W., Carruthers, J.R., Cooper, R.I., 
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 
 
Bruker Analytical X-ray Systems, Inc., 2006. Apex2, 
Version 2 User Manual, M86-E01078, Madison, WI. 
 
Prince, E. 
Mathematical Techniques in Crystallography 
and Materials Science 
Springer-Verlag, New York, 1982. 
 
Siemens Industrial Automation, Inc (1996). 
SADABS: Area-Detector Absorption Correction;: Madison, WI. 
 
Watkin D.J. (1994). 
Acta Cryst, A50, 411-437. 
 
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical 
Crystallography Laboratory, Oxford, UK. 
; 

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cu1 Cu 0.47513(12) 0.52487(12) 0.1565(5) 0.0454 1.0000 Uani DS T . . . . 
O1 O 0.4384(10) 0.4121(10) 0.2572(18) 0.077(3) 1.0000 Uiso D U . . . . 
O2 O 0.4812(11) 0.3715(10) -0.011(2) 0.079(3) 1.0000 Uiso D U . . . . 
O3 O 0.4350(6) 0.5650(6) 0.417(2) 0.049(6) 1.0000 Uiso DS . . . . . 
O4 O 0.2950(7) 0.0857(10) 0.809(2) 0.086(3) 1.0000 Uiso D U . . . . 
C1 C 0.4478(7) 0.3590(10) 0.162(2) 0.078(3) 1.0000 Uiso D U . . . . 
C2 C 0.4220(7) 0.2763(10) 0.261(2) 0.079(3) 1.0000 Uiso D U . . . . 
C3 C 0.3811(8) 0.2562(11) 0.446(3) 0.080(3) 1.0000 Uiso D U . . . . 
C4 C 0.3584(8) 0.1792(4) 0.536(3) 0.082(3) 1.0000 Uiso DS U . . . . 
C5 C 0.4404(9) 0.2202(4) 0.169(3) 0.079(3) 1.0000 Uiso DS U . . . . 
C6 C 0.3148(8) 0.1574(4) 0.730(3) 0.084(3) 1.0000 Uiso DS U . . . . 
C7 C 0.2519(11) 0.0578(16) 0.997(5) 0.086(4) 0.5000 Uiso D U . . . . 
H31 H 0.3680 0.2958 0.5112 0.0877 1.0000 Uiso . . . . . . 
H51 H 0.4692 0.2346 0.0447 0.0866 1.0000 Uiso . . . . . . 
H71 H 0.2408 0.0000 1.0000 0.0918 1.0000 Uiso D . . . . . 
H72 H 0.2812 0.0941 1.1049 0.0918 0.5000 Uiso D . . . . . 
H73 H 0.1956 0.0523 0.9906 0.0918 0.5000 Uiso D . . . . . 
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.047(3) 0.047(3) 0.060(2) 0.0000(10) 0.0000(10) 0.038(3) 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 0.158(3) 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
Cu1 . O1 11_665 1.937(15)    yes
Cu1 . O2 12_555 1.908(16)    yes
Cu1 . O2 2_665 1.908(16)    yes
Cu1 . Cu1 2_665 2.603(7)    yes
Cu1 . O1 . 1.937(15)    yes
Cu1 . O3 . 2.140(17)    yes
O1 . C1 . 1.24(2)    yes
O2 . C1 . 1.260(19)    yes
O4 . C6 . 1.283(18)    yes
O4 . C7 . 1.43(3)    yes
C1 . C2 . 1.49(2)    yes
C2 . C3 . 1.39(2)    yes
C2 . C5 . 1.37(2)    yes
C3 . C4 . 1.39(2)    yes
C3 . H31 . 0.969    no
C4 . C6 . 1.46(3)    yes
C5 . H51 . 0.942    no
C7 . H71 . 0.970    no
C7 . H72 . 0.938    no
C7 . H73 . 0.982    no
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
O1 11_665 Cu1 . O2 12_555 168.3(6)    yes
O1 11_665 Cu1 . O2 2_665 89.2(7)    yes
O2 12_555 Cu1 . O2 2_665 89.6(10)    yes
O1 11_665 Cu1 . Cu1 2_665 84.2(4)    yes
O2 12_555 Cu1 . Cu1 2_665 84.0(5)    yes
O2 2_665 Cu1 . Cu1 2_665 84.0(5)    yes
O1 11_665 Cu1 . O1 . 89.6(10)    yes
O2 12_555 Cu1 . O1 . 89.2(7)    yes
O2 2_665 Cu1 . O1 . 168.3(6)    yes
Cu1 2_665 Cu1 . O1 . 84.2(4)    yes
O1 11_665 Cu1 . O3 . 95.2(5)    yes
O2 12_555 Cu1 . O3 . 96.5(6)    yes
O2 2_665 Cu1 . O3 . 96.5(6)    yes
Cu1 2_665 Cu1 . O3 . 179.2(5)    yes
O1 . Cu1 . O3 . 95.2(5)    yes
Cu1 . O1 . C1 . 123.0(8)    yes
Cu1 2_665 O2 . C1 . 124.3(10)    yes
C6 . O4 . C7 . 123.2(8)    yes
O2 . C1 . O1 . 124.4(12)    yes
O2 . C1 . C2 . 117.4(8)    yes
O1 . C1 . C2 . 118.1(11)    yes
C1 . C2 . C3 . 120.8(9)    yes
C1 . C2 . C5 . 119.5(8)    yes
C3 . C2 . C5 . 119.6(8)    yes
C2 . C3 . C4 . 119.9(7)    yes
C2 . C3 . H31 . 119.9    no
C4 . C3 . H31 . 120.2    no
C3 . C4 . C3 9_555 119.5(12)    yes
C3 . C4 . C6 . 120.2(6)    yes
C3 9_555 C4 . C6 . 120.2(6)    yes
C2 . C5 . C2 9_555 121.2(13)    yes
C2 . C5 . H51 . 119.3    no
C2 9_555 C5 . H51 . 119.3    no
C4 . C6 . O4 . 118.5(7)    yes
C4 . C6 . O4 9_555 118.5(7)    yes
O4 . C6 . O4 9_555 123.0(14)    yes
O4 . C7 . H71 . 100.6    no
O4 . C7 . H72 . 113.2    no
H71 . C7 . H72 . 119.2    no
O4 . C7 . H73 . 111.1    no
H71 . C7 . H73 . 104.5    no
H72 . C7 . H73 . 107.8    no
C7 . H71 . C7 8_557 140.9    no
loop_
 _geom_hbond_atom_site_label_D
 _geom_hbond_site_symmetry_D
 _geom_hbond_atom_site_label_H
 _geom_hbond_site_symmetry_H
 _geom_hbond_atom_site_label_A
 _geom_hbond_site_symmetry_A
 _geom_hbond_angle_DHA
 _geom_hbond_distance_DH
 _geom_hbond_distance_HA
 _geom_hbond_distance_DA
 _geom_hbond_publ_flag
C7 . H71 . O4 8_557 137.3(19) 0.970 1.865 2.66(2)    yes
C7 8_557 H71 . O4 . 137.3(19) 0.970 1.865 2.66(2)    yes
C7 8_557 H71 . C7 . 141(2) 0.970 0.970 1.83(2)    yes
C7 . H72 . C2 9_556 134.7(14) 0.938 2.478 3.21(2)    yes


_iucr_refine_instruction_details_constraints
;
#
# Punched on 29/04/13 at 14:14:27
#
#LIST     12                                                                    
BLOCK 
CONT SCALE 
CONT CU   (    1 ,X'S,U'S) 
CONT O    (    1 ,X'S,U[ISO])  UNTIL C    (    7 ) 
END                                                                             
;


_iucr_refine_instruction_details_restraints
;
#
# Punched on 29/04/13 at 14:14:27
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = O(1) TO C(1) 
VIBR .0, 0.00200 = O(2) TO C(1) 
VIBR .0, 0.00200 = C(1) TO C(2) 
VIBR .0, 0.00500 = O(1) TO O(2) 
VIBR .0, 0.00500 = C(2) TO O(2) 
VIBR .0, 0.00500 = C(2) TO O(1) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00200 = C(2) TO C(5) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00500 = C(5) TO C(1) 
VIBR .0, 0.00500 = C(5) TO C(3) 
VIBR .0, 0.00200 = O(4) TO C(6) 
VIBR .0, 0.00200 = O(4) TO C(7) 
VIBR .0, 0.00500 = C(7) TO C(6) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00200 = C(6) TO C(4) 
VIBR .0, 0.00500 = O(4) TO O(4,5,1,0,1) 
VIBR .0, 0.00500 = C(4) TO O(4,5,1,0,1) 
VIBR .0, 0.00500 = C(4) TO O(4) 
VIBR .0, 0.00500 = C(2,5,1,0,1) TO C(2) 
VIBR .0, 0.00500 = C(3) TO C(6) 
VIBR .0, 0.00500 = C(3,5,1,0,1) TO C(6) 
VIBR .0, 0.00500 = C(3,5,1,0,1) TO C(3) 
VIBR .0, 0.00200 = C(7) TO C(7,-4,1,1,2,-1) 
VIBR .0, 0.00500 = O(4) TO C(7,-4,1,1,2,-1) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.08000 = O(1) TO C(1) 
U(IJ) .0, 0.08000 = O(2) TO C(1) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(2) TO C(5) 
U(IJ) .0, 0.04000 = O(4) TO C(6) 
U(IJ) .0, 0.04000 = O(4) TO C(7) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(6) TO C(4) 
U(IJ) .0, 0.04000 = C(7) TO C(7,-4,1,1,2,-1) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
DISTANCE 2.150000 , 0.050000 = CU(1) TO O(3) 
DISTANCE 1.950000 , 0.050000 = CU(1) TO O(1) 
DISTANCE 1.250000 , 0.050000 = O(1) TO C(1) 
DISTANCE 1.250000 , 0.050000 = C(1) TO O(2) 
DISTANCE 1.490000 , 0.050000 = C(1) TO C(2) 
DISTANCE 1.400000 , 0.050000 = C(2) TO C(5) 
DISTANCE 1.400000 , 0.050000 = C(2) TO C(3) 
DISTANCE 1.400000 , 0.050000 = C(3) TO C(4) 
DISTANCE 1.510000 , 0.050000 = C(4) TO C(6) 
DISTANCE 1.260000 , 0.050000 = C(6) TO O(4) 
DISTANCE 1.430000 , 0.050000 = O(4) TO C(7) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(71) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(72) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(73) 
ANGLE 94.800000 , 1.000000 = O(3) TO CU(1) TO O(1) 
ANGLE 123.000000 , 1.000000 = CU(1) TO O(1) TO C(1) 
ANGLE 120.000000 , 1.000000 = C(1) TO C(2) TO C(5) 
ANGLE 120.000000 , 1.000000 = C(5) TO C(2) TO C(3) 
ANGLE 120.000000 , 1.000000 = C(2) TO C(3) TO C(4) 
ANGLE 120.000000 , 1.000000 = C(3) TO C(4) TO C(6) 
ANGLE 118.000000 , 1.000000 = C(4) TO C(6) TO O(4) 
ANGLE 124.000000 , 1.000000 = C(6) TO O(4) TO C(7) 
ANGLE 118.000000 , 1.000000 = O(2) TO C(1) TO C(2) 
PLANAR 0.010000  C(1) C(2) C(5) C(3) C(4) C(6) O(4) C(7) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
  -3   4   4  x   .
 -12  12   2  x   .


#===END

data_ST1015
_audit_creation_date        "13-04-29"
_audit_creation_method CRYSTALS_ver_14.40

_oxford_structure_analysis_title  'ST2044 in P-3m1'
_chemical_name_systematic         ?
_chemical_melting_point           ?

#looking for refcif 
 
_publ_contact_author_name         'Scott C. McKellar' 
_publ_contact_author_address 
; 
 Dr Scott C. McKellar 
 The University of Edinburgh 
 Joseph Black Building 
 West Mains Road 
 Edinburgh 
 EH9 3JJ 
; 
 
_publ_contact_author_phone        '+44(0)131 6504804' 
_publ_contact_author_email        'smckella@staffmail.ed.ac.uk' 
; 

#==============================================================================
>>> The Following Model ALERTS were generated                 - (Acta-Mode) <<<
#==============================================================================
     
023_ALERT_3_A Resolution (too) Low [sin(theta)/Lambda < 0.6]..      17.20 Deg.
027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............      13.07 Deg.
088_ALERT_3_A Poor Data / Parameter Ratio ....................       5.04
029_ALERT_3_B _diffrn_measured_fraction_theta_full Low .......       0.94
341_ALERT_3_B Low Bond Precision on  C-C Bonds (x 1000) Ang ..         30
911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L=  0.416         38
022_ALERT_3_C Ratio Unique / Expected Reflections (too) Low ..       0.91
910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) .....          3
913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....         12
909_ALERT_3_G Percentage of Observed Data at Theta(Max) still          39 Perc.
950_ALERT_5_G Reported and Calculated Hmax Values Differ by ..          2

The high pressure cell causes shading of a significant proportion of the
sphere of reflections. This means that the completeness is reduced and as
such the quality of the model is lower.All of the above are cause by shading 
by the pressure cell.

020_ALERT_3_C The value of Rint is greater than 0.12 .........       0.16
082_ALERT_2_C High R1 Value ..................................       0.12
960_ALERT_3_G Number of Intensities with I .LT. - 2*sig(I) ..           2

These are caused by weak data and low completeness


601_ALERT_2_A Structure Contains Solvent Accessible VOIDS of .        223 A**3

Structure is a porous framework with disordered solvent in the pores.
The solvent region was treated by the van der Sluis and Spek method 
SQUEEZE), accounting for 105 e/cell. See below. This corresponds to 1 molecule
of acetaldehyde  in the large pore and 0.5 molecule of acetaldehyde in each small 
pore, per formula unit. F(000), M, mu, D and the given formulae have been 
calculated on this assumption.


201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) .......         10

Due to the low number of reflections available, all atoms (except Cu) were 
refined isotropically to maximise the data:parameter ratio. 


042_ALERT_1_C Calc. and Reported MoietyFormula Strings  Differ          ?

This is due to the disordered solvent present in the framework pores. The 
solvent was not able to be modelled and thus was handled using SQUEEZE as 
outlined above. 


045_ALERT_1_C Calculated and Reported Z Differ by ............       3.00 Ratio

This reflects the choice of forumla unit.


152_ALERT_1_C The Supplied and Calc. Volume s.u. Differ by ...         14 Units

This is due to rounding errors.


241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         O1

O1 is adjacent to a heavy atom (Cu1).


334_ALERT_2_C Small Average Benzene  C-C Dist. C2     -C5            1.37 Ang.

This has ben restrained to 1.4


732_ALERT_1_C Angle   Calc   122.8(17), Rep    122.9(8) ......       2.13 su-Ra
              CU1  -O1   -C1      1.555   1.555   1.555      #         16
732_ALERT_1_C Angle   Calc   117.7(19), Rep    117.6(8) ......       2.38 su-Ra
              O2   -C1   -C2      1.555   1.555   1.555      #         20
732_ALERT_1_C Angle   Calc   119.4(18), Rep    119.3(8) ......       2.25 su-Ra
              C1   -C2   -C5      1.555   1.555   1.555      #         23
732_ALERT_1_C Angle   Calc   119.3(18), Rep    119.4(8) ......       2.25 su-Ra
              C3   -C2   -C5      1.555   1.555   1.555      #         24
732_ALERT_1_C Angle   Calc      119(2), Rep    119.5(7) ......       2.86 su-Ra
              C2   -C3   -C4      1.555   1.555   1.555      #         25
752_ALERT_4_C Angle   Calc      119.99, Rep    120.1(6) ......  Senseless su
              C3   -C4   -C6      1.555   1.555   1.555      #         29

The use of restraints in the refinement mean that off diagonal terms in the
variance-covariance matrix are significant, and the diagonal approximation
used in Platon/Checkcif is badly in error.



004_ALERT_5_G Info: Polymeric Structure Found with Dimension .          1
760_ALERT_1_G CIF Contains no Torsion Angles .................          ?

No action taken.


301_ALERT_3_G Note: Main Residue  Disorder ...................          5 Perc.

Ester groups are disordered over two sites.


808_ALERT_5_G No Parseable SHELXL Style Weighting Scheme Found          !

A Shelx weighting scheme was not used

860_ALERT_3_G Note: Number of Least-Squares Restraints .......         53

Thermal similarity, vibration, distance and angle restraints required due to 
disorder and low completeness. 


929_ALERT_5_G No Weight Pars,Obs and Calc R1,wR2,S not checked          !

These have been included

#==============================================================================
;

loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000 -0.084       218        55 ' '
   2  0.333  0.667  0.005       111        25 ' '
   3  0.667  0.333 -0.051       111        25 ' '
_platon_squeeze_details
;
See above for details
;

 
_publ_section_exptl_refinement 
; 
; 
 
_publ_section_exptl_prep 
# Brief details or a reference. Include solvent if known 
; 
? 
; 
 
#end of refcif 
_cell_length_a                    17.991(3)
_cell_length_b                    17.991(3)
_cell_length_c                    6.5371(11)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      1832.5(5)
 
_symmetry_cell_setting            'trigonal' 
_symmetry_space_group_name_H-M    'P -3 m 1 ' 
_symmetry_space_group_name_Hall   '-P 3 2' 
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 '-x,-y,-z'
 '-y,x-y,z'
 'y,-x+y,-z'
 '-x+y,-x,z'
 'x-y,x,-z'
 '-x+y,y,z'
 'x-y,-y,-z'
 'x,x-y,z'
 '-x,-x+y,-z'
 '-y,-x,z'
 'y,x,-z'

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source  
 C       0.0033   0.0016   2.3100  20.8439   1.0200  10.2075   1.5886   0.5687
   0.8650  51.6512   0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 H       0.0000   0.0000   0.4930  10.5109   0.3229  26.1257   0.1402   3.1424
   0.0408  57.7998   0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 O       0.0106   0.0060   3.0485  13.2771   2.2868   5.7011   1.5463   0.3239
   0.8670  32.9089   0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 Cu      0.3201   1.2651  13.3380   3.5828   7.1676   0.2470   5.6158  11.3966
   1.6735  64.8126   1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 
 
_cell_formula_units_Z                    2

# Given Formula = C34 H32.00 Cu3 O23.00 
# Dc =      1.81 Fooo =    906.00 Mu =     18.22 M =    166.54
# Found Formula = C30 H18 Cu3 O21 
# Dc =      1.64 FOOO =    906.00 Mu =     18.09 M =    150.85

_chemical_formula_sum             'C34 H32.00 Cu3 O23.00'
_chemical_formula_moiety          'C30 H24 Cu3 O21 .2CH3CHO'
_chemical_compound_source                ?
_chemical_formula_weight            999.24
 
 
_cell_measurement_reflns_used          582
_cell_measurement_theta_min              3
_cell_measurement_theta_max             16
_cell_measurement_temperature          300
 
_exptl_crystal_description        'rod' 
_exptl_crystal_colour             'blue' 
_exptl_crystal_size_min           0.030 
_exptl_crystal_size_mid           0.040 
_exptl_crystal_size_max           0.100 
 
_exptl_crystal_density_diffrn     1.811 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              1014.00 
_exptl_absorpt_coefficient_mu     1.82 
 
# Sheldrick geometric approximatio 0.93 0.95 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'SADABS (Siemens, 1996)' 
_exptl_absorpt_correction_T_min   0.66 
_exptl_absorpt_correction_T_max   0.95 
_diffrn_measurement_device_type   'Bruker Kappa Apex2' 
_diffrn_measurement_device        'Area' 
_diffrn_radiation_monochromator   'graphite' 
_diffrn_radiation_type            'Mo K\a'
_diffrn_radiation_wavelength           0.71073
_diffrn_measurement_method        ω/2θ 
 
# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection        'Apex2 (Bruker AXS, 2006)' 
_computing_cell_refinement        'Apex2 (Bruker AXS, 2006)' 
_computing_data_reduction         'Apex2 (Bruker AXS, 2006)' 
_computing_structure_solution     'SIR92 (Altomare et al., 1994)' 
_computing_structure_refinement   'CRYSTALS (Betteridge et al., 2003)' 
_computing_publication_material   'CRYSTALS (Betteridge et al., 2003)' 
_computing_molecular_graphics     'CAMERON (Watkin et al., 1996)' 
 
_diffrn_standards_interval_time   . 
_diffrn_standards_interval_count  . 
_diffrn_standards_number          0 
_diffrn_standards_decay_%         ? 
 
_diffrn_ambient_temperature        300
_diffrn_ambient_pressure          3.0 #GPa
_diffrn_reflns_number             4194 
_reflns_number_total              389 
_diffrn_reflns_av_R_equivalents   0.159 
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 389 
# Theoretical number of reflections is about 737 
 
 
_diffrn_reflns_theta_min          3.116 
_diffrn_reflns_theta_max          17.202 
_diffrn_measured_fraction_theta_max 0.908 
 
_diffrn_reflns_theta_full         13.073 
_diffrn_measured_fraction_theta_full 0.942 
 
 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        0 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        5 
_reflns_limit_h_min               -12 
_reflns_limit_h_max               0 
_reflns_limit_k_min               0 
_reflns_limit_k_max               14 
_reflns_limit_l_min               0 
_reflns_limit_l_max               5 
 
_oxford_diffrn_Wilson_B_factor    5.04 
_oxford_diffrn_Wilson_scale       54.73 
 
_atom_sites_solution_primary      direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    difmap
 
_refine_diff_density_min          -0.61 
_refine_diff_density_max          0.73 
 
 
# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 
 
 
# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref     I>2.0\s(I)
_refine_ls_number_reflns          237 
_refine_ls_number_restraints      53 
_refine_ls_number_parameters      47 
_oxford_refine_ls_R_factor_ref    0.1204 
_refine_ls_wR_factor_ref          0.1342 
_refine_ls_goodness_of_fit_ref    1.1803 
_refine_ls_shift/su_max           0.0093316 
_refine_ls_shift/su_mean          0.0011208 
 
 
# The values computed with all filters except I/sigma 
_oxford_reflns_number_all         379 
_refine_ls_R_factor_all           0.1868 
_refine_ls_wR_factor_all          0.2319 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0σ(I)
_reflns_number_gt                 237 
_refine_ls_R_factor_gt            0.1204 
_refine_ls_wR_factor_gt           0.1342 
 
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration  '.' 
 
 
_refine_ls_structure_factor_coef  F 
_refine_ls_matrix_type            full
_refine_ls_hydrogen_treatment     noref          #undef, noref, refall,
                                                 # refxyz, refU, constr or mixed
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 1.25 0.335 0.599 
;
# Insert your own references if required - in alphabetical order 
_publ_section_references 
; 
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., 
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. 
 
Betteridge, P.W., Carruthers, J.R., Cooper, R.I., 
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 
 
Bruker Analytical X-ray Systems, Inc., 2006. Apex2, 
Version 2 User Manual, M86-E01078, Madison, WI. 
 
Prince, E. 
Mathematical Techniques in Crystallography 
and Materials Science 
Springer-Verlag, New York, 1982. 
 
Siemens Industrial Automation, Inc (1996). 
SADABS: Area-Detector Absorption Correction;: Madison, WI. 
 
Watkin D.J. (1994). 
Acta Cryst, A50, 411-437. 
 
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical 
Crystallography Laboratory, Oxford, UK. 
; 

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cu1 Cu 0.47388(18) 0.52612(18) 0.1552(7) 0.0749 1.0000 Uani DS T . . . . 
O1 O 0.4342(14) 0.4105(13) 0.262(3) 0.116(5) 1.0000 Uiso D U . . . . 
O2 O 0.4793(16) 0.3690(14) -0.002(3) 0.117(5) 1.0000 Uiso D U . . . . 
O3 O 0.4330(7) 0.5670(7) 0.417(3) 0.065(9) 1.0000 Uiso DS . . . . . 
O4 O 0.2934(8) 0.0857(12) 0.838(3) 0.121(5) 1.0000 Uiso D U . . . . 
C1 C 0.4462(8) 0.3575(12) 0.172(3) 0.117(5) 1.0000 Uiso D U . . . . 
C2 C 0.4198(8) 0.2754(12) 0.273(3) 0.117(5) 1.0000 Uiso D U . . . . 
C3 C 0.3804(9) 0.2566(14) 0.466(4) 0.118(5) 1.0000 Uiso D U . . . . 
C4 C 0.3566(9) 0.1783(5) 0.556(4) 0.119(5) 1.0000 Uiso DS U . . . . 
C5 C 0.4341(10) 0.2170(5) 0.180(4) 0.117(5) 1.0000 Uiso DS U . . . . 
C6 C 0.3141(9) 0.1570(4) 0.762(3) 0.120(5) 1.0000 Uiso DS U . . . . 
C7 C 0.2518(12) 0.0574(17) 1.038(5) 0.121(6) 0.5000 Uiso D U . . . . 
H31 H 0.3699 0.2980 0.5340 0.1374 1.0000 Uiso . . . . . . 
H51 H 0.4561 0.2280 0.0444 0.1361 1.0000 Uiso . . . . . . 
H71 H 0.2420 0.0014 1.0654 0.1392 0.5000 Uiso D . . . . . 
H72 H 0.2879 0.0960 1.1392 0.1392 0.5000 Uiso D . . . . . 
H73 H 0.1988 0.0566 1.0343 0.1392 0.5000 Uiso D . . . . . 
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.095(5) 0.095(5) 0.074(4) 0.0031(17) -0.0031(17) 0.077(5) 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 0.163(3) 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
Cu1 . O1 11_665 1.96(2)    yes
Cu1 . O2 2_665 1.92(2)    yes
Cu1 . O2 12_555 1.92(2)    yes
Cu1 . Cu1 2_665 2.601(10)    yes
Cu1 . O1 . 1.96(2)    yes
Cu1 . O3 . 2.14(2)    yes
O1 . C1 . 1.23(2)    yes
O2 . C1 . 1.25(2)    yes
O4 . C6 . 1.25(2)    yes
O4 . C7 . 1.46(3)    yes
C1 . C2 . 1.46(2)    yes
C2 . C3 . 1.40(3)    yes
C2 . C5 . 1.35(2)    yes
C3 . C4 . 1.38(3)    yes
C3 . H31 . 0.965    no
C4 . C6 . 1.50(3)    yes
C5 . H51 . 0.949    no
C7 . H71 8_557 1.184    no
C7 . H71 . 0.951    no
C7 . H72 . 0.944    no
C7 . H73 . 0.946    no
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
O1 11_665 Cu1 . O2 2_665 87.9(10)    yes
O1 11_665 Cu1 . O2 12_555 167.8(8)    yes
O2 2_665 Cu1 . O2 12_555 90.6(15)    yes
O1 11_665 Cu1 . Cu1 2_665 84.3(5)    yes
O2 2_665 Cu1 . Cu1 2_665 83.6(7)    yes
O2 12_555 Cu1 . Cu1 2_665 83.6(7)    yes
O1 11_665 Cu1 . O1 . 91.0(14)    yes
O2 2_665 Cu1 . O1 . 167.8(8)    yes
O2 12_555 Cu1 . O1 . 87.9(10)    yes
Cu1 2_665 Cu1 . O1 . 84.3(5)    yes
O1 11_665 Cu1 . O3 . 94.2(6)    yes
O2 2_665 Cu1 . O3 . 97.9(8)    yes
O2 12_555 Cu1 . O3 . 97.9(8)    yes
Cu1 2_665 Cu1 . O3 . 177.8(7)    yes
O1 . Cu1 . O3 . 94.2(6)    yes
Cu1 . O1 . C1 . 122.9(8)    yes
Cu1 2_665 O2 . C1 . 125.1(14)    yes
C6 . O4 . C7 . 123.4(8)    yes
O2 . C1 . O1 . 124.0(14)    yes
O2 . C1 . C2 . 117.6(8)    yes
O1 . C1 . C2 . 118.3(13)    yes
C1 . C2 . C3 . 121.3(10)    yes
C1 . C2 . C5 . 119.3(8)    yes
C3 . C2 . C5 . 119.4(8)    yes
C2 . C3 . C4 . 119.5(7)    yes
C2 . C3 . H31 . 120.0    no
C4 . C3 . H31 . 120.6    no
C3 . C4 . C3 9_555 119.4(13)    yes
C3 . C4 . C6 . 120.1(6)    yes
C3 9_555 C4 . C6 . 120.1(6)    yes
C2 9_555 C5 . C2 . 122.2(15)    yes
C2 9_555 C5 . H51 . 118.9    no
C2 . C5 . H51 . 118.9    no
C4 . C6 . O4 . 118.1(7)    yes
C4 . C6 . O4 9_555 118.1(7)    yes
O4 . C6 . O4 9_555 123.3(14)    yes
O4 . C7 . H71 8_557 68.4    no
O4 . C7 . H71 . 109.2    no
H71 8_557 C7 . H71 . 45.7    no
O4 . C7 . H72 . 109.0    no
H71 8_557 C7 . H72 . 143.4    no
H71 . C7 . H72 . 109.9    no
O4 . C7 . H73 . 108.7    no
H71 8_557 C7 . H73 . 104.6    no
H71 . C7 . H73 . 109.7    no
H72 . C7 . H73 . 110.3    no
C7 8_557 H71 . C7 . 120.5    no
loop_
 _geom_hbond_atom_site_label_D
 _geom_hbond_site_symmetry_D
 _geom_hbond_atom_site_label_H
 _geom_hbond_site_symmetry_H
 _geom_hbond_atom_site_label_A
 _geom_hbond_site_symmetry_A
 _geom_hbond_angle_DHA
 _geom_hbond_distance_DH
 _geom_hbond_distance_HA
 _geom_hbond_distance_DA
 _geom_hbond_publ_flag
C3 . H31 . O1 12_556 155.5(8) 0.965 2.554 3.46(3)    yes
C7 . H71 . O4 8_557 161(2) 0.951 1.505 2.42(3)    yes
C7 . H71 . C7 8_557 120.5(11) 0.951 1.184 1.86(3)    yes
C7 . H72 . C2 9_556 139.5(16) 0.944 2.257 3.04(3)    yes
C7 . H72 . C3 9_556 149.1(18) 0.944 2.597 3.44(3)    yes
C7 . H72 . C5 1_556 140(2) 0.944 2.450 3.23(3)    yes


_iucr_refine_instruction_details_constraints
;
#
# Punched on 29/04/13 at 14:32:40
#
#LIST     12                                                                    
BLOCK 
CONT SCALE 
CONT CU   (    1 ,X'S,U'S) 
CONT O    (    1 ,X'S,U[ISO])  UNTIL C    (    7 ) 
END                                                                             
;


_iucr_refine_instruction_details_restraints
;
#
# Punched on 29/04/13 at 14:32:40
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = O(1) TO C(1) 
VIBR .0, 0.00200 = O(2) TO C(1) 
VIBR .0, 0.00200 = C(1) TO C(2) 
VIBR .0, 0.00500 = O(1) TO O(2) 
VIBR .0, 0.00500 = C(2) TO O(2) 
VIBR .0, 0.00500 = C(2) TO O(1) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00200 = C(2) TO C(5) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00500 = C(5) TO C(1) 
VIBR .0, 0.00500 = C(5) TO C(3) 
VIBR .0, 0.00200 = O(4) TO C(6) 
VIBR .0, 0.00200 = O(4) TO C(7) 
VIBR .0, 0.00500 = C(7) TO C(6) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00200 = C(6) TO C(4) 
VIBR .0, 0.00500 = O(4) TO O(4,5,1,0,1) 
VIBR .0, 0.00500 = C(4) TO O(4,5,1,0,1) 
VIBR .0, 0.00500 = C(4) TO O(4) 
VIBR .0, 0.00500 = C(2,5,1,0,1) TO C(2) 
VIBR .0, 0.00500 = C(3) TO C(6) 
VIBR .0, 0.00500 = C(3,5,1,0,1) TO C(6) 
VIBR .0, 0.00500 = C(3,5,1,0,1) TO C(3) 
VIBR .0, 0.00200 = C(7) TO C(7,-4,1,1,2,-1) 
VIBR .0, 0.00500 = O(4) TO C(7,-4,1,1,2,-1) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.08000 = O(1) TO C(1) 
U(IJ) .0, 0.08000 = O(2) TO C(1) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(2) TO C(5) 
U(IJ) .0, 0.04000 = O(4) TO C(6) 
U(IJ) .0, 0.04000 = O(4) TO C(7) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(6) TO C(4) 
U(IJ) .0, 0.04000 = C(7) TO C(7,-4,1,1,2,-1) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
DISTANCE 2.150000 , 0.050000 = CU(1) TO O(3) 
DISTANCE 1.950000 , 0.050000 = CU(1) TO O(1) 
DISTANCE 1.250000 , 0.050000 = O(1) TO C(1) 
DISTANCE 1.250000 , 0.050000 = C(1) TO O(2) 
DISTANCE 1.490000 , 0.050000 = C(1) TO C(2) 
DISTANCE 1.400000 , 0.050000 = C(2) TO C(5) 
DISTANCE 1.400000 , 0.050000 = C(2) TO C(3) 
DISTANCE 1.400000 , 0.050000 = C(3) TO C(4) 
DISTANCE 1.510000 , 0.050000 = C(4) TO C(6) 
DISTANCE 1.260000 , 0.050000 = C(6) TO O(4) 
DISTANCE 1.430000 , 0.050000 = O(4) TO C(7) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(71) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(72) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(73) 
ANGLE 94.800000 , 1.000000 = O(3) TO CU(1) TO O(1) 
ANGLE 123.000000 , 1.000000 = CU(1) TO O(1) TO C(1) 
ANGLE 120.000000 , 1.000000 = C(1) TO C(2) TO C(5) 
ANGLE 120.000000 , 1.000000 = C(5) TO C(2) TO C(3) 
ANGLE 120.000000 , 1.000000 = C(2) TO C(3) TO C(4) 
ANGLE 120.000000 , 1.000000 = C(3) TO C(4) TO C(6) 
ANGLE 118.000000 , 1.000000 = C(4) TO C(6) TO O(4) 
ANGLE 124.000000 , 1.000000 = C(6) TO O(4) TO C(7) 
ANGLE 118.000000 , 1.000000 = O(2) TO C(1) TO C(2) 
PLANAR 0.010000  C(1) C(2) C(5) C(3) C(4) C(6) O(4) C(7) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
  -3   4   4  x   .
 -12  12   2  x   .
  -1   4   0  x   .

#===END

data_HK1001 
_audit_creation_date        "13-05-02"
_audit_creation_method CRYSTALS_ver_14.40

_oxford_structure_analysis_title  'ST2009 in Fm-3m'
_chemical_name_systematic         ?
_chemical_melting_point           ?

#looking for refcif 
 
_publ_contact_author_name         'Scott C. McKellar' 
_publ_contact_author_address 
; 
 Dr Scott C. McKellar 
 The University of Edinburgh 
 Joseph Black Building 
 West Mains Road 
 Edinburgh 
 EH9 3JJ 
; 
 
_publ_contact_author_phone        '+44(0)131 6504804' 
_publ_contact_author_email        'smckella@staffmail.ed.ac.uk' 
;

#==============================================================================
>>> The Following Model ALERTS were generated                 - (Acta-Mode) <<<
 
601_ALERT_2_A Structure Contains Solvent Accessible VOIDS of .      11591 A**3

Structure is a porous framework with disordered water in the pores.
The solvent region was treated by the van der Sluis and Spek method (SQUEEZE), 
accounting for 1105 e/cell. See below. This corresponds to 7 molecules of water 
per formula unit. F(000), M, mu, D and the given formulae have been 
calculated on this assumption.


042_ALERT_1_C Calc. and Reported MoietyFormula Strings  Differ          ?

This is due to the disordered solvent present in the framework pores. 
The solvent was not able to be modelled and thus was handled using 
SQUEEZE as outlined above. 


045_ALERT_1_C Calculated and Reported Z Differ by ............       3.00 Ratio

This reflects the choice of forumla unit.


242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        Cu1

Cu1 is a heavy atom 

004_ALERT_5_G Info: Polymeric Structure Found with Dimension .          1
760_ALERT_1_G CIF Contains no Torsion Angles .................          ?
764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) .       1.11 Ratio
794_ALERT_5_G Note: Tentative Bond Valency for Cu1     (II)          2.15

Noted, no action taken


152_ALERT_1_G The Supplied and Calc. Volume s.u. Differ by ...          3 Units

This is due to rounding errors


808_ALERT_5_G No Parseable SHELXL Style Weighting Scheme Found          !

A Shelx weighting scheme was not used.


929_ALERT_5_G No Weight Pars,Obs and Calc R1,wR2,S not checked          !

These have been included


950_ALERT_5_G Reported and Calculated Hmax Values Differ by ..         14
951_ALERT_5_G Reported and Calculated Kmax Values Differ by ..          9
960_ALERT_3_G Number of Intensities with I .LT. - 2*sig(I) ..           1
910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) .....          6
913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....          1

This is due to weak data at high angle due to room temperature data
collection and porous nature of crystal. Data collection was also 
performed as a sphere, so was not optimised. Data is still 
99.4% complete (see below), and data was included to as high an angle 
as possible in the refinement.
Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged)

Theta sin(th)/Lambda Complete  Expected Measured  Missing
-------------------------------------------------------------------------------
 20.82     0.500     0.989          543      537        6
 23.01     0.550     0.990          702      695        7
 25.24     0.600     0.993          891      885        6
------------------------------------------------------------ ACTA Min. Res. ---
 26.35     0.624     0.994          995      989        6
#============================================================================== 
;
 
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.008 -0.031 -0.009     11615      1105 ' '
_platon_squeeze_details
;
see above for details
;
 
_publ_section_exptl_refinement 
; 
; 
 
_publ_section_exptl_prep 
# Brief details or a reference. Include solvent if known 
; 
? 
; 
 
#end of refcif 
_cell_length_a                    26.315(3)
_cell_length_b                    26.315(3)
_cell_length_c                    26.315(3)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      18223(3)
 
_symmetry_cell_setting            'cubic' 
_symmetry_space_group_name_H-M    'F m -3 m ' 
_symmetry_space_group_name_Hall   '-F 4 2 3' 
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 '-x,-y,-z'
 'x,y+1/2,z+1/2'
 '-x,-y+1/2,-z+1/2'
 'x+1/2,y,z+1/2'
 '-x+1/2,-y,-z+1/2'
 'x+1/2,y+1/2,z'
 '-x+1/2,-y+1/2,-z'
 'y,z,x'
 '-y,-z,-x'
 'y,z+1/2,x+1/2'
 '-y,-z+1/2,-x+1/2'
 'y+1/2,z,x+1/2'
 '-y+1/2,-z,-x+1/2'
 'y+1/2,z+1/2,x'
 '-y+1/2,-z+1/2,-x'
 'z,x,y'
 '-z,-x,-y'
 'z,x+1/2,y+1/2'
 '-z,-x+1/2,-y+1/2'
 'z+1/2,x,y+1/2'
 '-z+1/2,-x,-y+1/2'
 'z+1/2,x+1/2,y'
 '-z+1/2,-x+1/2,-y'
 'x,y,-z'
 '-x,-y,z'
 'x,y+1/2,-z+1/2'
 '-x,-y+1/2,z+1/2'
 'x+1/2,y,-z+1/2'
 '-x+1/2,-y,z+1/2'
 'x+1/2,y+1/2,-z'
 '-x+1/2,-y+1/2,z'
 'y,z,-x'
 '-y,-z,x'
 'y,z+1/2,-x+1/2'
 '-y,-z+1/2,x+1/2'
 'y+1/2,z,-x+1/2'
 '-y+1/2,-z,x+1/2'
 'y+1/2,z+1/2,-x'
 '-y+1/2,-z+1/2,x'
 'z,x,-y'
 '-z,-x,y'
 'z,x+1/2,-y+1/2'
 '-z,-x+1/2,y+1/2'
 'z+1/2,x,-y+1/2'
 '-z+1/2,-x,y+1/2'
 'z+1/2,x+1/2,-y'
 '-z+1/2,-x+1/2,y'
 'y,-z,-x'
 '-y,z,x'
 'y,-z+1/2,-x+1/2'
 '-y,z+1/2,x+1/2'
 'y+1/2,-z,-x+1/2'
 '-y+1/2,z,x+1/2'
 'y+1/2,-z+1/2,-x'
 '-y+1/2,z+1/2,x'
 'z,-x,-y'
 '-z,x,y'
 'z,-x+1/2,-y+1/2'
 '-z,x+1/2,y+1/2'
 'z+1/2,-x,-y+1/2'
 '-z+1/2,x,y+1/2'
 'z+1/2,-x+1/2,-y'
 '-z+1/2,x+1/2,y'
 '-z,x,-y'
 'z,-x,y'
 '-z,x+1/2,-y+1/2'
 'z,-x+1/2,y+1/2'
 '-z+1/2,x,-y+1/2'
 'z+1/2,-x,y+1/2'
 '-z+1/2,x+1/2,-y'
 'z+1/2,-x+1/2,y'
 '-x,y,-z'
 'x,-y,z'
 '-x,y+1/2,-z+1/2'
 'x,-y+1/2,z+1/2'
 '-x+1/2,y,-z+1/2'
 'x+1/2,-y,z+1/2'
 '-x+1/2,y+1/2,-z'
 'x+1/2,-y+1/2,z'
 '-y,z,-x'
 'y,-z,x'
 '-y,z+1/2,-x+1/2'
 'y,-z+1/2,x+1/2'
 '-y+1/2,z,-x+1/2'
 'y+1/2,-z,x+1/2'
 '-y+1/2,z+1/2,-x'
 'y+1/2,-z+1/2,x'
 'x,-y,-z'
 '-x,y,z'
 'x,-y+1/2,-z+1/2'
 '-x,y+1/2,z+1/2'
 'x+1/2,-y,-z+1/2'
 '-x+1/2,y,z+1/2'
 'x+1/2,-y+1/2,-z'
 '-x+1/2,y+1/2,z'
 'y,x,z'
 '-y,-x,-z'
 'y,x+1/2,z+1/2'
 '-y,-x+1/2,-z+1/2'
 'y+1/2,x,z+1/2'
 '-y+1/2,-x,-z+1/2'
 'y+1/2,x+1/2,z'
 '-y+1/2,-x+1/2,-z'
 'z,y,x'
 '-z,-y,-x'
 'z,y+1/2,x+1/2'
 '-z,-y+1/2,-x+1/2'
 'z+1/2,y,x+1/2'
 '-z+1/2,-y,-x+1/2'
 'z+1/2,y+1/2,x'
 '-z+1/2,-y+1/2,-x'
 'x,z,y'
 '-x,-z,-y'
 'x,z+1/2,y+1/2'
 '-x,-z+1/2,-y+1/2'
 'x+1/2,z,y+1/2'
 '-x+1/2,-z,-y+1/2'
 'x+1/2,z+1/2,y'
 '-x+1/2,-z+1/2,-y'
 'y,x,-z'
 '-y,-x,z'
 'y,x+1/2,-z+1/2'
 '-y,-x+1/2,z+1/2'
 'y+1/2,x,-z+1/2'
 '-y+1/2,-x,z+1/2'
 'y+1/2,x+1/2,-z'
 '-y+1/2,-x+1/2,z'
 'z,y,-x'
 '-z,-y,x'
 'z,y+1/2,-x+1/2'
 '-z,-y+1/2,x+1/2'
 'z+1/2,y,-x+1/2'
 '-z+1/2,-y,x+1/2'
 'z+1/2,y+1/2,-x'
 '-z+1/2,-y+1/2,x'
 'x,z,-y'
 '-x,-z,y'
 'x,z+1/2,-y+1/2'
 '-x,-z+1/2,y+1/2'
 'x+1/2,z,-y+1/2'
 '-x+1/2,-z,y+1/2'
 'x+1/2,z+1/2,-y'
 '-x+1/2,-z+1/2,y'
 '-z,y,-x'
 'z,-y,x'
 '-z,y+1/2,-x+1/2'
 'z,-y+1/2,x+1/2'
 '-z+1/2,y,-x+1/2'
 'z+1/2,-y,x+1/2'
 '-z+1/2,y+1/2,-x'
 'z+1/2,-y+1/2,x'
 '-x,z,-y'
 'x,-z,y'
 '-x,z+1/2,-y+1/2'
 'x,-z+1/2,y+1/2'
 '-x+1/2,z,-y+1/2'
 'x+1/2,-z,y+1/2'
 '-x+1/2,z+1/2,-y'
 'x+1/2,-z+1/2,y'
 'x,-z,-y'
 '-x,z,y'
 'x,-z+1/2,-y+1/2'
 '-x,z+1/2,y+1/2'
 'x+1/2,-z,-y+1/2'
 '-x+1/2,z,y+1/2'
 'x+1/2,-z+1/2,-y'
 '-x+1/2,z+1/2,y'
 'y,-x,-z'
 '-y,x,z'
 'y,-x+1/2,-z+1/2'
 '-y,x+1/2,z+1/2'
 'y+1/2,-x,-z+1/2'
 '-y+1/2,x,z+1/2'
 'y+1/2,-x+1/2,-z'
 '-y+1/2,x+1/2,z'
 'z,-y,-x'
 '-z,y,x'
 'z,-y+1/2,-x+1/2'
 '-z,y+1/2,x+1/2'
 'z+1/2,-y,-x+1/2'
 '-z+1/2,y,x+1/2'
 'z+1/2,-y+1/2,-x'
 '-z+1/2,y+1/2,x'
 '-y,x,-z'
 'y,-x,z'
 '-y,x+1/2,-z+1/2'
 'y,-x+1/2,z+1/2'
 '-y+1/2,x,-z+1/2'
 'y+1/2,-x,z+1/2'
 '-y+1/2,x+1/2,-z'
 'y+1/2,-x+1/2,z'

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source  
 C       0.0033   0.0016   2.3100  20.8439   1.0200  10.2075   1.5886   0.5687
   0.8650  51.6512   0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 H       0.0000   0.0000   0.4930  10.5109   0.3229  26.1257   0.1402   3.1424
   0.0408  57.7998   0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 O       0.0106   0.0060   3.0485  13.2771   2.2868   5.7011   1.5463   0.3239
   0.8670  32.9089   0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 Cu      0.3201   1.2651  13.3380   3.5828   7.1676   0.2470   5.6158  11.3966
   1.6735  64.8126   1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 
 
_cell_formula_units_Z                    16

# Given Formula = C18 H25.88 Cu3 O21.94 
# Dc =      1.14 Fooo =   5136.00 Mu =     14.47 M =     65.33
# Found Formula = C18 H6 Cu3 O15 
# Dc =      0.95 FOOO =   5136.00 Mu =     14.26 M =     54.41

_chemical_formula_sum             'C18 H26 Cu3 O22'
_chemical_formula_moiety          'C18 H12 Cu3 O15 .7(H2O)'
_chemical_compound_source                ?
_chemical_formula_weight            783.90
 
 
_cell_measurement_reflns_used          495
_cell_measurement_theta_min              4
_cell_measurement_theta_max             26
_cell_measurement_temperature          298
 
_exptl_crystal_description        'block' 
_exptl_crystal_colour             'blue' 
_exptl_crystal_size_min           0.200 
_exptl_crystal_size_mid           0.200 
_exptl_crystal_size_max           0.200 
 
_exptl_crystal_density_diffrn     1.143
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              6342 
_exptl_absorpt_coefficient_mu     1.45 
 
# Sheldrick geometric approximatio 0.75 0.75 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'SADABS (Siemens, 1996)' 
_exptl_absorpt_correction_T_min   0.64 
_exptl_absorpt_correction_T_max   0.75 
_diffrn_measurement_device_type   'Bruker Kappa Apex2' 
_diffrn_measurement_device        'Area' 
_diffrn_radiation_monochromator   'graphite' 
_diffrn_radiation_type            'Mo K\a'
_diffrn_radiation_wavelength           0.71073
_diffrn_measurement_method        ω/2θ 
 
# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection        'Apex2 (Bruker AXS, 2006)' 
_computing_cell_refinement        'Apex2 (Bruker AXS, 2006)' 
_computing_data_reduction         'Apex2 (Bruker AXS, 2006)' 
_computing_structure_solution     'SIR92 (Altomare et al., 1994)' 
_computing_structure_refinement   'CRYSTALS (Betteridge et al., 2003)' 
_computing_publication_material   'CRYSTALS (Betteridge et al., 2003)' 
_computing_molecular_graphics     'CAMERON (Watkin et al., 1996)' 
 
_diffrn_standards_interval_time   . 
_diffrn_standards_interval_count  . 
_diffrn_standards_number          0 
_diffrn_standards_decay_%         ? 
 
_diffrn_ambient_temperature        298
_diffrn_reflns_number             7111 
_reflns_number_total              989 
_diffrn_reflns_av_R_equivalents   0.033 
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 989 
# Theoretical number of reflections is about 1549 
 
 
_diffrn_reflns_theta_min          3.375 
_diffrn_reflns_theta_max          26.346 
_diffrn_measured_fraction_theta_max 0.994 
 
_diffrn_reflns_theta_full         26.346 
_diffrn_measured_fraction_theta_full 0.994 
 
 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        18 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        23 
_diffrn_reflns_limit_l_min        3 
_diffrn_reflns_limit_l_max        32 
_reflns_limit_h_min               0 
_reflns_limit_h_max               18 
_reflns_limit_k_min               0 
_reflns_limit_k_max               23 
_reflns_limit_l_min               3 
_reflns_limit_l_max               32 
 
_oxford_diffrn_Wilson_B_factor    1.68 
_oxford_diffrn_Wilson_scale       4618.97 
 
_atom_sites_solution_primary      direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    difmap
 
_refine_diff_density_min          -0.35 
_refine_diff_density_max          0.49 
 
 
# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 
 
 
# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref     I>-10.0\s(I)
_refine_ls_number_reflns          984 
_refine_ls_number_restraints      0 
_refine_ls_number_parameters      36 
_oxford_refine_ls_R_factor_ref    0.0397 
_refine_ls_wR_factor_ref          0.0896 
_refine_ls_goodness_of_fit_ref    0.9030 
_refine_ls_shift/su_max           0.0025950 
_refine_ls_shift/su_mean          0.0001285 
 
 
# The values computed with all filters except I/sigma 
_oxford_reflns_number_all         984 
_refine_ls_R_factor_all           0.0397 
_refine_ls_wR_factor_all          0.0896 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0σ(I)
_reflns_number_gt                 897 
_refine_ls_R_factor_gt            0.0354 
_refine_ls_wR_factor_gt           0.0879 
 
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration  '.' 
 
 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full
_refine_ls_hydrogen_treatment     noref          #undef, noref, refall,
                                                 # refxyz, refU, constr or mixed
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 8.23 13.3 7.61 3.03 0.658 
;
# Insert your own references if required - in alphabetical order 
_publ_section_references 
; 
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., 
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. 
 
Betteridge, P.W., Carruthers, J.R., Cooper, R.I., 
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 
 
Bruker Analytical X-ray Systems, Inc., 2006. Apex2, 
Version 2 User Manual, M86-E01078, Madison, WI. 
 
Prince, E. 
Mathematical Techniques in Crystallography 
and Materials Science 
Springer-Verlag, New York, 1982. 
 
Siemens Industrial Automation, Inc (1996). 
SADABS: Area-Detector Absorption Correction;: Madison, WI. 
 
Watkin D.J. (1994). 
Acta Cryst, A50, 411-437. 
 
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical 
Crystallography Laboratory, Oxford, UK. 
; 

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cu1 Cu 0.785344(12) 0.285344(12) 0.5000 0.0308 1.0000 Uani S T . . . . 
O1 O 0.84374(11) 0.34374(11) 0.5000 0.1033 1.0000 Uani S T . . . . 
O2 O 0.81701(6) 0.24328(6) 0.55253(6) 0.0506 1.0000 Uani . . . . . . 
C1 C 0.79683(9) 0.20317(9) 0.56912(11) 0.0407 1.0000 Uani S T . . . . 
C2 C 0.82221(8) 0.17779(8) 0.61311(11) 0.0389 1.0000 Uani S T . . . . 
C3 C 0.80089(12) 0.13465(9) 0.63465(9) 0.0419 1.0000 Uani S T . . . . 
H31 H 0.7702 0.1207 0.6207 0.0382 1.0000 Uiso . . . . . . 
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0328(2) 0.0328(2) 0.0268(3) 0.0000 0.0000 -0.01100(19) 
O1 0.086(2) 0.086(2) 0.139(5) 0.0000 0.0000 -0.055(3) 
O2 0.0526(9) 0.0516(10) 0.0476(9) 0.0148(8) -0.0146(7) -0.0138(8) 
C1 0.0444(10) 0.0444(10) 0.0333(14) 0.0036(9) -0.0036(9) -0.0026(13) 
C2 0.0410(10) 0.0410(10) 0.0348(14) 0.0054(9) -0.0054(9) -0.0025(12) 
C3 0.0407(16) 0.0426(10) 0.0426(10) 0.0022(13) -0.0054(10) -0.0054(10) 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 0.021115(3) 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
Cu1 . O2 127_546 1.9572(16)    yes
Cu1 . O2 103_545 1.9572(16)    yes
Cu1 . O2 25_556 1.9572(16)    yes
Cu1 . Cu1 122_665 2.6307(9)    yes
Cu1 . O1 . 2.173(4)    yes
Cu1 . O2 . 1.9572(16)    yes
O2 . C1 . 1.260(2)    yes
C1 . C2 . 1.494(4)    yes
C2 . C3 122_665 1.387(2)    yes
C2 . C3 . 1.387(2)    yes
C3 . H31 . 0.960    no
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
O2 127_546 Cu1 . O2 103_545 89.87(11)    yes
O2 127_546 Cu1 . O2 25_556 89.01(11)    yes
O2 103_545 Cu1 . O2 25_556 168.65(9)    yes
O2 127_546 Cu1 . Cu1 122_665 84.32(5)    yes
O2 103_545 Cu1 . Cu1 122_665 84.32(5)    yes
O2 25_556 Cu1 . Cu1 122_665 84.32(5)    yes
O2 127_546 Cu1 . O1 . 95.68(5)    yes
O2 103_545 Cu1 . O1 . 95.68(5)    yes
O2 25_556 Cu1 . O1 . 95.68(5)    yes
Cu1 122_665 Cu1 . O1 . 179.995    yes
O2 127_546 Cu1 . O2 . 168.65(9)    yes
O2 103_545 Cu1 . O2 . 89.01(11)    yes
O2 25_556 Cu1 . O2 . 89.87(11)    yes
Cu1 122_665 Cu1 . O2 . 84.32(5)    yes
O1 . Cu1 . O2 . 95.68(5)    yes
Cu1 . O2 . C1 . 122.63(16)    yes
O2 122_665 C1 . O2 . 125.9(3)    yes
O2 122_665 C1 . C2 . 117.04(14)    yes
O2 . C1 . C2 . 117.04(14)    yes
C1 . C2 . C3 122_665 120.10(15)    yes
C1 . C2 . C3 . 120.10(15)    yes
C3 122_665 C2 . C3 . 119.7(3)    yes
C2 . C3 . C2 83_646 120.3(3)    yes
C2 . C3 . H31 . 119.8    no
C2 83_646 C3 . H31 . 119.8    no


_iucr_refine_instruction_details_constraints
;
#
# Punched on 02/05/13 at 11:54:11
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
END                                                                             
;


_iucr_refine_instruction_details_restraints
;
#
# Punched on 02/05/13 at 11:54:11
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

#===END

data_HK1002
_audit_creation_date        "13-06-03"
_audit_creation_method CRYSTALS_ver_14.40

_oxford_structure_analysis_title  'ST2010_reprocess in Fm-3m'
_chemical_name_systematic         ?
_chemical_melting_point           ?

#looking for refcif 
 
_publ_contact_author_name         'Scott C. McKellar' 
_publ_contact_author_address 
; 
 Dr Scott C. McKellar 
 The University of Edinburgh 
 Joseph Black Building 
 West Mains Road 
 Edinburgh 
 EH9 3JJ 
; 
 
_publ_contact_author_phone        '+44(0)131 6504804' 
_publ_contact_author_email        'smckella@staffmail.ed.ac.uk' 
; 
 
#==============================================================================
>>> The Following Model ALERTS were generated                 - (Acta-Mode) <<<
#==============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
023_ALERT_3_A Resolution (too) Low [sin(theta)/Lambda < 0.6]..      18.94 Deg.
027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............      16.67 Deg.
088_ALERT_3_C Poor Data / Parameter Ratio ....................       8.03
341_ALERT_3_C Low Bond Precision on  C-C Bonds (x 1000) Ang ..         10
910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) .....          5
911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.457          6
913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....         10
950_ALERT_5_G Reported and Calculated Hmax Values Differ by ..         11
951_ALERT_5_G Reported and Calculated Kmax Values Differ by ..          7
909_ALERT_3_G Percentage of Observed Data at Theta(Max) still          37 Perc.

The high pressure cell causes shading of a significant proportion of the
sphere of reflections. This means that the completeness is reduced and as
such the quality of the model is lower.All of the above are cause by shading 
by the pressure cell.


601_ALERT_2_A Structure Contains Solvent Accessible VOIDS of .      11685 A**3

Structure is a porous framework with disordered solvent in the pores.
The solvent region was treated by the van der Sluis and Spek method 
(SQUEEZE), accounting for 2061 e/cell. This equates to 13 water molecules 
per formula unit. See below. F(000), M, mu, D and the given formulae have
been calculated on this assumption.


042_ALERT_1_C Calc. and Reported MoietyFormula Strings  Differ          ?

This is due to the disordered solvent present in the framework pores. The 
solvent was not able to be modelled and thus was handled using SQUEEZE as 
outlined above.


045_ALERT_1_C Calculated and Reported Z Differ by ............       3.00 Ratio

This reflects the choice of forumla unit.


242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        Cu1

Cu1 is a heavy atom.

152_ALERT_1_G The Supplied and Calc. Volume s.u. Differ by ...          2 Units

This is due to rounding errors


004_ALERT_5_G Info: Polymeric Structure Found with Dimension .          1
180_ALERT_4_G Check Cell Rounding: # of Values Ending with 0 =          3
760_ALERT_1_G CIF Contains no Torsion Angles .................          ?
764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) .       1.11 Ratio
794_ALERT_5_G Note: Tentative Bond Valency for Cu1     (II)          2.21

No action taken.


808_ALERT_5_G No Parseable SHELXL Style Weighting Scheme Found          !

A Shelx weighting scheme was not used


860_ALERT_3_G Note: Number of Least-Squares Restraints .......         36

Thermal similarity and vibration restraints required due to 
disorder and low completeness. 


929_ALERT_5_G No Weight Pars,Obs and Calc R1,wR2,S not checked          !

These have been included
#==============================================================================
;

loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.007 -0.027 -0.008     11816      2061 ' '
_platon_squeeze_details
;
see above for details
;

_publ_section_exptl_refinement 
; 
; 
 
_publ_section_exptl_prep 
# Brief details or a reference. Include solvent if known 
; 
? 
; 
 
#end of refcif 
_cell_length_a                    26.370(3)
_cell_length_b                    26.370(3)
_cell_length_c                    26.370(3)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      18337(4)
 
_symmetry_cell_setting            'cubic' 
_symmetry_space_group_name_H-M    'F m -3 m ' 
_symmetry_space_group_name_Hall   '-F 4 2 3' 
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 '-x,-y,-z'
 'x,y+1/2,z+1/2'
 '-x,-y+1/2,-z+1/2'
 'x+1/2,y,z+1/2'
 '-x+1/2,-y,-z+1/2'
 'x+1/2,y+1/2,z'
 '-x+1/2,-y+1/2,-z'
 'y,z,x'
 '-y,-z,-x'
 'y,z+1/2,x+1/2'
 '-y,-z+1/2,-x+1/2'
 'y+1/2,z,x+1/2'
 '-y+1/2,-z,-x+1/2'
 'y+1/2,z+1/2,x'
 '-y+1/2,-z+1/2,-x'
 'z,x,y'
 '-z,-x,-y'
 'z,x+1/2,y+1/2'
 '-z,-x+1/2,-y+1/2'
 'z+1/2,x,y+1/2'
 '-z+1/2,-x,-y+1/2'
 'z+1/2,x+1/2,y'
 '-z+1/2,-x+1/2,-y'
 'x,y,-z'
 '-x,-y,z'
 'x,y+1/2,-z+1/2'
 '-x,-y+1/2,z+1/2'
 'x+1/2,y,-z+1/2'
 '-x+1/2,-y,z+1/2'
 'x+1/2,y+1/2,-z'
 '-x+1/2,-y+1/2,z'
 'y,z,-x'
 '-y,-z,x'
 'y,z+1/2,-x+1/2'
 '-y,-z+1/2,x+1/2'
 'y+1/2,z,-x+1/2'
 '-y+1/2,-z,x+1/2'
 'y+1/2,z+1/2,-x'
 '-y+1/2,-z+1/2,x'
 'z,x,-y'
 '-z,-x,y'
 'z,x+1/2,-y+1/2'
 '-z,-x+1/2,y+1/2'
 'z+1/2,x,-y+1/2'
 '-z+1/2,-x,y+1/2'
 'z+1/2,x+1/2,-y'
 '-z+1/2,-x+1/2,y'
 'y,-z,-x'
 '-y,z,x'
 'y,-z+1/2,-x+1/2'
 '-y,z+1/2,x+1/2'
 'y+1/2,-z,-x+1/2'
 '-y+1/2,z,x+1/2'
 'y+1/2,-z+1/2,-x'
 '-y+1/2,z+1/2,x'
 'z,-x,-y'
 '-z,x,y'
 'z,-x+1/2,-y+1/2'
 '-z,x+1/2,y+1/2'
 'z+1/2,-x,-y+1/2'
 '-z+1/2,x,y+1/2'
 'z+1/2,-x+1/2,-y'
 '-z+1/2,x+1/2,y'
 '-z,x,-y'
 'z,-x,y'
 '-z,x+1/2,-y+1/2'
 'z,-x+1/2,y+1/2'
 '-z+1/2,x,-y+1/2'
 'z+1/2,-x,y+1/2'
 '-z+1/2,x+1/2,-y'
 'z+1/2,-x+1/2,y'
 '-x,y,-z'
 'x,-y,z'
 '-x,y+1/2,-z+1/2'
 'x,-y+1/2,z+1/2'
 '-x+1/2,y,-z+1/2'
 'x+1/2,-y,z+1/2'
 '-x+1/2,y+1/2,-z'
 'x+1/2,-y+1/2,z'
 '-y,z,-x'
 'y,-z,x'
 '-y,z+1/2,-x+1/2'
 'y,-z+1/2,x+1/2'
 '-y+1/2,z,-x+1/2'
 'y+1/2,-z,x+1/2'
 '-y+1/2,z+1/2,-x'
 'y+1/2,-z+1/2,x'
 'x,-y,-z'
 '-x,y,z'
 'x,-y+1/2,-z+1/2'
 '-x,y+1/2,z+1/2'
 'x+1/2,-y,-z+1/2'
 '-x+1/2,y,z+1/2'
 'x+1/2,-y+1/2,-z'
 '-x+1/2,y+1/2,z'
 'y,x,z'
 '-y,-x,-z'
 'y,x+1/2,z+1/2'
 '-y,-x+1/2,-z+1/2'
 'y+1/2,x,z+1/2'
 '-y+1/2,-x,-z+1/2'
 'y+1/2,x+1/2,z'
 '-y+1/2,-x+1/2,-z'
 'z,y,x'
 '-z,-y,-x'
 'z,y+1/2,x+1/2'
 '-z,-y+1/2,-x+1/2'
 'z+1/2,y,x+1/2'
 '-z+1/2,-y,-x+1/2'
 'z+1/2,y+1/2,x'
 '-z+1/2,-y+1/2,-x'
 'x,z,y'
 '-x,-z,-y'
 'x,z+1/2,y+1/2'
 '-x,-z+1/2,-y+1/2'
 'x+1/2,z,y+1/2'
 '-x+1/2,-z,-y+1/2'
 'x+1/2,z+1/2,y'
 '-x+1/2,-z+1/2,-y'
 'y,x,-z'
 '-y,-x,z'
 'y,x+1/2,-z+1/2'
 '-y,-x+1/2,z+1/2'
 'y+1/2,x,-z+1/2'
 '-y+1/2,-x,z+1/2'
 'y+1/2,x+1/2,-z'
 '-y+1/2,-x+1/2,z'
 'z,y,-x'
 '-z,-y,x'
 'z,y+1/2,-x+1/2'
 '-z,-y+1/2,x+1/2'
 'z+1/2,y,-x+1/2'
 '-z+1/2,-y,x+1/2'
 'z+1/2,y+1/2,-x'
 '-z+1/2,-y+1/2,x'
 'x,z,-y'
 '-x,-z,y'
 'x,z+1/2,-y+1/2'
 '-x,-z+1/2,y+1/2'
 'x+1/2,z,-y+1/2'
 '-x+1/2,-z,y+1/2'
 'x+1/2,z+1/2,-y'
 '-x+1/2,-z+1/2,y'
 '-z,y,-x'
 'z,-y,x'
 '-z,y+1/2,-x+1/2'
 'z,-y+1/2,x+1/2'
 '-z+1/2,y,-x+1/2'
 'z+1/2,-y,x+1/2'
 '-z+1/2,y+1/2,-x'
 'z+1/2,-y+1/2,x'
 '-x,z,-y'
 'x,-z,y'
 '-x,z+1/2,-y+1/2'
 'x,-z+1/2,y+1/2'
 '-x+1/2,z,-y+1/2'
 'x+1/2,-z,y+1/2'
 '-x+1/2,z+1/2,-y'
 'x+1/2,-z+1/2,y'
 'x,-z,-y'
 '-x,z,y'
 'x,-z+1/2,-y+1/2'
 '-x,z+1/2,y+1/2'
 'x+1/2,-z,-y+1/2'
 '-x+1/2,z,y+1/2'
 'x+1/2,-z+1/2,-y'
 '-x+1/2,z+1/2,y'
 'y,-x,-z'
 '-y,x,z'
 'y,-x+1/2,-z+1/2'
 '-y,x+1/2,z+1/2'
 'y+1/2,-x,-z+1/2'
 '-y+1/2,x,z+1/2'
 'y+1/2,-x+1/2,-z'
 '-y+1/2,x+1/2,z'
 'z,-y,-x'
 '-z,y,x'
 'z,-y+1/2,-x+1/2'
 '-z,y+1/2,x+1/2'
 'z+1/2,-y,-x+1/2'
 '-z+1/2,y,x+1/2'
 'z+1/2,-y+1/2,-x'
 '-z+1/2,y+1/2,x'
 '-y,x,-z'
 'y,-x,z'
 '-y,x+1/2,-z+1/2'
 'y,-x+1/2,z+1/2'
 '-y+1/2,x,-z+1/2'
 'y+1/2,-x,z+1/2'
 '-y+1/2,x+1/2,-z'
 'y+1/2,-x+1/2,z'

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source  
 C       0.0033   0.0016   2.3100  20.8439   1.0200  10.2075   1.5886   0.5687
   0.8650  51.6512   0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 H       0.0000   0.0000   0.4930  10.5109   0.3229  26.1257   0.1402   3.1424
   0.0408  57.7998   0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 O       0.0106   0.0060   3.0485  13.2771   2.2868   5.7011   1.5463   0.3239
   0.8670  32.9089   0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 Cu      0.3201   1.2651  13.3380   3.5828   7.1676   0.2470   5.6158  11.3966
   1.6735  64.8126   1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 
 
_cell_formula_units_Z                    16

# Given Formula = C18 H37.75 Cu3 O27.88 
# Dc =      1.29 Fooo =   5136.00 Mu =     14.55 M =     74.24
# Found Formula = C18 H6 Cu3 O15 
# Dc =      0.95 FOOO =   5136.00 Mu =     14.17 M =     54.41

_chemical_formula_sum             'C18 H38 Cu3 O28'
_chemical_formula_moiety          'C18 H12 Cu3 O15 .13(H2O)'
_chemical_compound_source                ?
_chemical_formula_weight            890.813
 
 
_cell_measurement_reflns_used         1060
_cell_measurement_theta_min              3
_cell_measurement_theta_max             23
_cell_measurement_temperature          298
 
_exptl_crystal_description        'block' 
_exptl_crystal_colour             'blue' 
_exptl_crystal_size_min           0.200 
_exptl_crystal_size_mid           0.200 
_exptl_crystal_size_max           0.200 
 
_exptl_crystal_density_diffrn     1.291 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              7292 
_exptl_absorpt_coefficient_mu     1.46 
 
# Sheldrick geometric approximatio 0.75 0.75 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'SADABS (Siemens, 1996)' 
_exptl_absorpt_correction_T_min   0.33 
_exptl_absorpt_correction_T_max   0.75 
_diffrn_measurement_device_type   'Bruker Kappa Apex2' 
_diffrn_measurement_device        'Area' 
_diffrn_radiation_monochromator   'graphite' 
_diffrn_radiation_type            'Mo K\a'
_diffrn_radiation_wavelength           0.71073
_diffrn_measurement_method        ω 
 
# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection        'Apex2 (Bruker AXS, 2006)' 
_computing_cell_refinement        'Apex2 (Bruker AXS, 2006)' 
_computing_data_reduction         'Apex2 (Bruker AXS, 2006)' 
_computing_structure_solution     'SIR92 (Altomare et al., 1994)' 
_computing_structure_refinement   'CRYSTALS (Betteridge et al., 2003)' 
_computing_publication_material   'CRYSTALS (Betteridge et al., 2003)' 
_computing_molecular_graphics     'CAMERON (Watkin et al., 1996)' 
 
_diffrn_standards_interval_time   . 
_diffrn_standards_interval_count  . 
_diffrn_standards_number          0 
_diffrn_standards_decay_%         ? 
 
_diffrn_ambient_temperature        298
_diffrn_ambient_pressure          0.2 #GPa
_diffrn_reflns_number             5734 
_reflns_number_total              411 
_diffrn_reflns_av_R_equivalents   0.188 
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 411 
# Theoretical number of reflections is about 603 
 
 
_diffrn_reflns_theta_min          3.090 
_diffrn_reflns_theta_max          18.938 
_diffrn_measured_fraction_theta_max 0.972 
 
_diffrn_reflns_theta_full         16.666 
_diffrn_measured_fraction_theta_full 0.982 
 
 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        17 
_diffrn_reflns_limit_l_min        3 
_diffrn_reflns_limit_l_max        23 
_reflns_limit_h_min               0 
_reflns_limit_h_max               13 
_reflns_limit_k_min               0 
_reflns_limit_k_max               17 
_reflns_limit_l_min               3 
_reflns_limit_l_max               23 
 
_oxford_diffrn_Wilson_B_factor    1.56 
_oxford_diffrn_Wilson_scale       3904.34 
 
_atom_sites_solution_primary      direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    difmap
 
_refine_diff_density_min          -0.66 
_refine_diff_density_max          0.29 
 
 
# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 
 
 
# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref     I>2.0\s(I)
_refine_ls_number_reflns          289 
_refine_ls_number_restraints      36 
_refine_ls_number_parameters      36 
_oxford_refine_ls_R_factor_ref    0.0510 
_refine_ls_wR_factor_ref          0.0556 
_refine_ls_goodness_of_fit_ref    1.0750 
_refine_ls_shift/su_max           0.0006501 
_refine_ls_shift/su_mean          0.0000481 
 
 
# The values computed with all filters except I/sigma 
_oxford_reflns_number_all         405 
_refine_ls_R_factor_all           0.0764 
_refine_ls_wR_factor_all          0.0869 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0σ(I)
_reflns_number_gt                 289 
_refine_ls_R_factor_gt            0.0510 
_refine_ls_wR_factor_gt           0.0556 
 
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration  '.' 
 
 
_refine_ls_structure_factor_coef  F 
_refine_ls_matrix_type            full
_refine_ls_hydrogen_treatment     noref          #undef, noref, refall,
                                                 # refxyz, refU, constr or mixed
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.615 0.490 0.375 
;
# Insert your own references if required - in alphabetical order 
_publ_section_references 
; 
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., 
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. 
 
Betteridge, P.W., Carruthers, J.R., Cooper, R.I., 
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 
 
Bruker Analytical X-ray Systems, Inc., 2006. Apex2, 
Version 2 User Manual, M86-E01078, Madison, WI. 
 
Prince, E. 
Mathematical Techniques in Crystallography 
and Materials Science 
Springer-Verlag, New York, 1982. 
 
Siemens Industrial Automation, Inc (1996). 
SADABS: Area-Detector Absorption Correction;: Madison, WI. 
 
Watkin D.J. (1994). 
Acta Cryst, A50, 411-437. 
 
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical 
Crystallography Laboratory, Oxford, UK. 
; 

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cu1 Cu 0.78505(4) 0.28505(4) 0.5000 0.0462 1.0000 Uani S T . . . . 
O1 O 0.8433(3) 0.3433(3) 0.5000 0.1036 1.0000 Uani S T . . . . 
O2 O 0.81682(17) 0.24368(18) 0.55219(17) 0.0638 1.0000 Uani . U . . . . 
C1 C 0.7966(3) 0.2034(3) 0.5700(3) 0.0551 1.0000 Uani S TU . . . . 
C2 C 0.8227(2) 0.1773(2) 0.6134(3) 0.0503 1.0000 Uani DS TU . . . . 
C3 C 0.8013(4) 0.1346(2) 0.6346(2) 0.0515 1.0000 Uani DS TU . . . . 
H31 H 0.7702 0.1207 0.6207 0.0382 1.0000 Uiso . . . . . . 
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0484(10) 0.0484(10) 0.0419(12) 0.0000 0.0000 -0.0083(9) 
O1 0.097(5) 0.097(5) 0.116(9) 0.0000 0.0000 -0.039(7) 
O2 0.062(3) 0.075(3) 0.055(3) 0.015(2) -0.005(2) -0.011(3) 
C1 0.063(4) 0.063(4) 0.038(6) 0.001(2) -0.001(2) -0.006(4) 
C2 0.055(4) 0.055(4) 0.040(5) 0.000(2) 0.000(2) -0.006(4) 
C3 0.061(7) 0.047(3) 0.047(3) -0.005(4) -0.011(3) -0.011(3) 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 0.02201(17) 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
Cu1 . O2 127_546 1.946(4)    yes
Cu1 . O2 103_545 1.946(4)    yes
Cu1 . O2 25_556 1.946(4)    yes
Cu1 . Cu1 122_665 2.614(3)    yes
Cu1 . O1 . 2.172(10)    yes
Cu1 . O2 . 1.946(4)    yes
O2 . C1 . 1.278(6)    yes
C1 . C2 . 1.502(12)    yes
C2 . C3 46_665 1.379(6)    yes
C2 . C3 . 1.379(6)    yes
C3 . H31 . 0.970    no
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
O2 127_546 Cu1 . O2 103_545 90.0(3)    yes
O2 127_546 Cu1 . O2 25_556 89.0(3)    yes
O2 103_545 Cu1 . O2 25_556 169.4(3)    yes
O2 127_546 Cu1 . Cu1 122_665 84.72(14)    yes
O2 103_545 Cu1 . Cu1 122_665 84.72(14)    yes
O2 25_556 Cu1 . Cu1 122_665 84.72(14)    yes
O2 127_546 Cu1 . O1 . 95.28(14)    yes
O2 103_545 Cu1 . O1 . 95.28(14)    yes
O2 25_556 Cu1 . O1 . 95.28(14)    yes
Cu1 122_665 Cu1 . O1 . 179.995    yes
O2 127_546 Cu1 . O2 . 169.4(3)    yes
O2 103_545 Cu1 . O2 . 89.0(3)    yes
O2 25_556 Cu1 . O2 . 90.0(3)    yes
Cu1 122_665 Cu1 . O2 . 84.72(14)    yes
O1 . Cu1 . O2 . 95.28(14)    yes
Cu1 . O2 . C1 . 123.1(5)    yes
O2 122_665 C1 . O2 . 124.0(9)    yes
O2 122_665 C1 . C2 . 118.0(4)    yes
O2 . C1 . C2 . 118.0(4)    yes
C1 . C2 . C3 46_665 119.7(5)    yes
C1 . C2 . C3 . 119.7(5)    yes
C3 46_665 C2 . C3 . 120.3(9)    yes
C2 . C3 . C2 115_545 119.7(9)    yes
C2 . C3 . H31 . 120.1    no
C2 115_545 C3 . H31 . 120.1    no


_iucr_refine_instruction_details_constraints
;
#
# Punched on 03/06/13 at 11:53:01
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
END                                                                             
;


_iucr_refine_instruction_details_restraints
;
#
# Punched on 03/06/13 at 11:53:01
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = O(2) TO C(1) 
VIBR .0, 0.00200 = C(1) TO C(2) 
VIBR .0, 0.00500 = O(2,-16,1,1,1) TO O(2) 
VIBR .0, 0.00500 = C(2) TO O(2) 
VIBR .0, 0.00500 = C(2) TO O(2,-16,1,1,1) 
VIBR .0, 0.00200 = C(2) TO C(3,-6,3,1,1) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00500 = C(3,-6,3,1,1) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(3,-6,3,1,1) 
VIBR .0, 0.00500 = C(2,11,2,1,-1,1) TO C(2) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = O(2) TO C(1) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.04000 = C(2) TO C(3,-6,3,1,1) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
DISTANCE 1.400000 , 0.050000 = C(2) TO C(3) 
END                                                                             
;



















