# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Pent_029_Lab
_database_code_depnum_ccdc_archive 'CCDC 1564952'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2020-06-09 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_audit_creation_date             2017-05-19
_audit_creation_method           CRYSTALS_ver_14.61_build_6236

_oxford_structure_analysis_title 'ST6119_0m in R-3'
_chemical_name_systematic        ?
_chemical_melting_point          ?

#end of refcif 
_cell_length_a                   26.038(3)
_cell_length_b                   26.038(3)
_cell_length_c                   7.7843(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4570.4(10)

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3

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            9

# Given Formula = C10 H10 Cu1 N1 O2 
# Dc =      1.57 Fooo =   2196.00 Mu =     21.21 M =    239.74
# Found Formula = C9 H8 Cu0.50 N1 O2 
# Dc =      1.27 FOOO =   1791.00 Mu =     10.96 M =    193.94

_chemical_formula_sum            'C18 H16 Cu N2 O4'
_chemical_formula_moiety         'C18 H16 Cu N2 O4'
_chemical_compound_source        ?
_chemical_formula_weight         193.94


_cell_measurement_reflns_used    1047
_cell_measurement_theta_min      3
_cell_measurement_theta_max      19
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1791
_exptl_absorpt_coefficient_mu    1.096

# Sheldrick geometric approximatio 0.80 0.90 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_T_max  0.90
_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            3353
_reflns_number_total             675
_diffrn_reflns_av_R_equivalents  0.065
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 675 
# Theoretical number of reflections is about 1601 


_diffrn_reflns_theta_min         3.129
_diffrn_reflns_theta_max         18.861
_diffrn_measured_fraction_theta_max 0.838

_diffrn_reflns_theta_full        14.146
_diffrn_measured_fraction_theta_full 0.871


_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       6
_reflns_limit_h_min              -23
_reflns_limit_h_max              10
_reflns_limit_k_min              0
_reflns_limit_k_max              23
_reflns_limit_l_min              0
_reflns_limit_l_max              6

_oxford_diffrn_Wilson_B_factor   4.29
_oxford_diffrn_Wilson_scale      5466.96

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.65
_refine_diff_density_max         0.89


# 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         670
_refine_ls_number_restraints     126
_refine_ls_number_parameters     115
_oxford_refine_ls_R_factor_ref   0.1054
_refine_ls_wR_factor_ref         0.2639
_refine_ls_goodness_of_fit_ref   0.9777
_refine_ls_shift/su_max          0.0000774
_refine_ls_shift/su_mean         0.0000114


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        670
_refine_ls_R_factor_all          0.1054
_refine_ls_wR_factor_all         0.2639

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                493
_refine_ls_R_factor_gt           0.0785
_refine_ls_wR_factor_gt          0.2168

# 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) + ( 0.15P)² +*****P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# 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 0.8333 0.6667 0.6667 0.0537 1.0000 Uani S . . . . .
O2 O 0.7600(4) 0.6349(4) 0.5283(11) 0.0607 1.0000 Uani D U . . . .
C4 C 0.7111(4) 0.5890(5) 0.5669(13) 0.0637 1.0000 Uani D U . . . .
C5 C 0.6620(4) 0.5723(6) 0.4390(11) 0.0552 1.0000 Uani D U . . . .
C6 C 0.6749(4) 0.5935(7) 0.2724(13) 0.0812 1.0000 Uani D U . . . .
C7 C 0.6305(5) 0.5731(7) 0.1518(12) 0.0787 1.0000 Uani D U . . . .
N1 N 0.5739(4) 0.5360(5) 0.1879(12) 0.0686 1.0000 Uani D U . . . .
C9 C 0.5614(4) 0.5179(6) 0.3508(13) 0.0648 1.0000 Uani D U . . . .
C8 C 0.6028(4) 0.5344(7) 0.4769(12) 0.0707 1.0000 Uani D U . . . .
C3 C 0.7000(4) 0.5546(6) 0.7113(14) 0.0700 1.0000 Uani D U . . . .
C2 C 0.7421(4) 0.5558(6) 0.8260(16) 0.0741 1.0000 Uani D U . . . .
O1 O 0.7967(4) 0.5914(5) 0.8209(11) 0.0676 1.0000 Uani D U . . . .
C1 C 0.7205(7) 0.5069(7) 0.957(2) 0.1100 1.0000 Uani D U . . . .
H61 H 0.7145 0.6205 0.2382 0.1022 1.0000 Uiso R . . . . .
H71 H 0.6407 0.5878 0.0378 0.0896 1.0000 Uiso R . . . . .
H91 H 0.5207 0.4933 0.3793 0.0936 1.0000 Uiso R . . . . .
H81 H 0.5906 0.5192 0.5897 0.0964 1.0000 Uiso R . . . . .
H31 H 0.6593 0.5275 0.7330 0.0946 1.0000 Uiso R . . . . .
H11 H 0.7544 0.5060 1.0088 0.1381 1.0000 Uiso R . . . . .
H12 H 0.6988 0.5148 1.0456 0.1381 1.0000 Uiso R . . . . .
H13 H 0.6942 0.4685 0.9029 0.1381 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.017501(7)
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 . N1 9_655 2.218(8) yes
Cu1 . N1 10_555 2.218(8) yes
Cu1 . O1 6_666 2.080(10) yes
Cu1 . O2 6_666 1.978(9) yes
Cu1 . O2 . 1.978(9) yes
Cu1 . O1 . 2.080(10) yes
O2 . C4 . 1.271(7) yes
C4 . C5 . 1.503(7) yes
C4 . C3 . 1.375(8) yes
C5 . C6 . 1.384(8) yes
C5 . C8 . 1.384(8) yes
C6 . C7 . 1.373(8) yes
C6 . H61 . 0.950 no
C7 . N1 . 1.327(8) yes
C7 . H71 . 0.950 no
N1 . C9 . 1.335(8) yes
C9 . C8 . 1.360(8) yes
C9 . H91 . 0.950 no
C8 . H81 . 0.950 no
C3 . C2 . 1.403(8) yes
C3 . H31 . 0.950 no
C2 . O1 . 1.250(8) yes
C2 . C1 . 1.501(8) yes
C1 . H11 . 0.980 no
C1 . H12 . 0.979 no
C1 . H13 . 0.979 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
N1 9_655 Cu1 . N1 10_555 179.995 yes
N1 9_655 Cu1 . O1 6_666 93.3(4) yes
N1 10_555 Cu1 . O1 6_666 86.7(4) yes
N1 9_655 Cu1 . O2 6_666 89.4(4) yes
N1 10_555 Cu1 . O2 6_666 90.6(4) yes
O1 6_666 Cu1 . O2 6_666 91.6(4) yes
N1 9_655 Cu1 . O2 . 90.6(4) yes
N1 10_555 Cu1 . O2 . 89.4(4) yes
O1 6_666 Cu1 . O2 . 88.4(4) yes
O2 6_666 Cu1 . O2 . 179.994 yes
N1 9_655 Cu1 . O1 . 86.7(4) yes
N1 10_555 Cu1 . O1 . 93.3(4) yes
O1 6_666 Cu1 . O1 . 179.994 yes
O2 6_666 Cu1 . O1 . 88.4(4) yes
O2 . Cu1 . O1 . 91.6(4) yes
Cu1 . O2 . C4 . 124.6(6) yes
O2 . C4 . C5 . 115.0(5) yes
O2 . C4 . C3 . 126.2(6) yes
C5 . C4 . C3 . 118.8(5) yes
C4 . C5 . C6 . 120.2(5) yes
C4 . C5 . C8 . 123.3(5) yes
C6 . C5 . C8 . 116.5(5) yes
C5 . C6 . C7 . 119.8(6) yes
C5 . C6 . H61 . 121.0 no
C7 . C6 . H61 . 119.1 no
C6 . C7 . N1 . 123.4(6) yes
C6 . C7 . H71 . 118.1 no
N1 . C7 . H71 . 118.4 no
Cu1 16_545 N1 . C7 . 125.5(6) yes
Cu1 16_545 N1 . C9 . 118.1(6) yes
C7 . N1 . C9 . 116.4(6) yes
N1 . C9 . C8 . 124.0(6) yes
N1 . C9 . H91 . 116.9 no
C8 . C9 . H91 . 119.0 no
C5 . C8 . C9 . 119.7(6) yes
C5 . C8 . H81 . 121.0 no
C9 . C8 . H81 . 119.2 no
C4 . C3 . C2 . 126.8(6) yes
C4 . C3 . H31 . 114.9 no
C2 . C3 . H31 . 118.3 no
C3 . C2 . O1 . 125.6(6) yes
C3 . C2 . C1 . 117.1(6) yes
O1 . C2 . C1 . 117.1(6) yes
C2 . O1 . Cu1 . 122.2(6) yes
C2 . C1 . H11 . 109.8 no
C2 . C1 . H12 . 108.2 no
H11 . C1 . H12 . 109.4 no
C2 . C1 . H13 . 110.5 no
H11 . C1 . H13 . 109.5 no
H12 . C1 . H13 . 109.4 no



# 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
-19 16 1 x .
-5 6 4 x .
# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 
# looking for PLATON_SQD.SQF 

# SQUEEZE RESULTS (Version =  60516) 
# Note: Data are Listed for all Voids in the P1 Unit Cell 
# i.e. Centre of Gravity, Solvent Accessible Volume, 
# Recovered number of Electrons in the Void and 
# Details about the Squeezed Material 
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 -0.011 356 132 ' '
2 0.333 0.667 -0.178 361 132 ' '
3 0.667 0.333 0.110 362 133 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_MeOH_096_Syn
_database_code_depnum_ccdc_archive 'CCDC 1564955'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2020-06-09 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_audit_creation_date             2016-06-08
_audit_creation_method           CRYSTALS_ver_14.61_build_5965

_oxford_structure_analysis_title 'LATE02_0m in R-3'
_chemical_name_systematic        ?
_chemical_melting_point          ?

#end of refcif 
_cell_length_a                   26.025(2)
_cell_length_b                   26.025(2)
_cell_length_c                   7.7498(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4545.7(8)

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3

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            9

# Given Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.28 Fooo =   1791.00 Mu =     11.02 M =    387.88
# Found Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.28 FOOO =   1791.00 Mu =     11.02 M =    387.88

_chemical_formula_sum            'C18 H16 Cu1 N2 O4'
_chemical_formula_moiety         'C18 H16 Cu1 N2 O4'
_chemical_compound_source        ?
_chemical_formula_weight         387.88


_cell_measurement_reflns_used    1907
_cell_measurement_theta_min      2
_cell_measurement_theta_max      16
_cell_measurement_temperature    293

_exptl_crystal_description       green
_exptl_crystal_colour            block
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1791
_exptl_absorpt_coefficient_mu    1.102

# Sheldrick geometric approximatio 0.80 0.90 
_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  0.90
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_device       Serial
_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       'USER DEFINED DATA COLLECTION'
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_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_ambient_pressure         960000
_diffrn_reflns_number            4147
_reflns_number_total             1181
_diffrn_reflns_av_R_equivalents  0.059
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 1181 
# Theoretical number of reflections is about 2890 


_diffrn_reflns_theta_min         2.779
_diffrn_reflns_theta_max         23.223
_diffrn_measured_fraction_theta_max 0.814

_diffrn_reflns_theta_full        22.759
_diffrn_measured_fraction_theta_full 0.816


_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_reflns_limit_h_min              -28
_reflns_limit_h_max              11
_reflns_limit_k_min              0
_reflns_limit_k_max              28
_reflns_limit_l_min              0
_reflns_limit_l_max              8

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.76
_refine_diff_density_max         0.75


# 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>-3.0\s(I)
_refine_ls_number_reflns         1173
_refine_ls_number_restraints     126
_refine_ls_number_parameters     115
_oxford_refine_ls_R_factor_ref   0.1035
_refine_ls_wR_factor_ref         0.2525
_refine_ls_goodness_of_fit_ref   1.0556
_refine_ls_shift/su_max          0.0000931
_refine_ls_shift/su_mean         0.0000161


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1173
_refine_ls_R_factor_all          0.1035
_refine_ls_wR_factor_all         0.2525

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                889
_refine_ls_R_factor_gt           0.0823
_refine_ls_wR_factor_gt          0.2171

# 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, 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: 
 5.36 6.63 1.90 
;

# 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 0.8333 0.6667 0.6667 0.0376 1.0000 Uani S . . . . .
O2 O 0.7599(2) 0.6345(3) 0.5308(7) 0.0452 1.0000 Uani D U . . . .
C4 C 0.7097(3) 0.5920(3) 0.5776(8) 0.0457 1.0000 Uani D U . . . .
C5 C 0.6608(3) 0.5746(3) 0.4480(7) 0.0451 1.0000 Uani D U . . . .
C6 C 0.6746(3) 0.5957(4) 0.2801(9) 0.0591 1.0000 Uani D U . . . .
C7 C 0.6306(3) 0.5760(4) 0.1569(9) 0.0592 1.0000 Uani D U . . . .
N1 N 0.5742(3) 0.5372(3) 0.1897(8) 0.0526 1.0000 Uani D U . . . .
C9 C 0.5613(3) 0.5181(4) 0.3527(8) 0.0537 1.0000 Uani D U . . . .
C8 C 0.6019(3) 0.5359(4) 0.4837(8) 0.0507 1.0000 Uani D U . . . .
C3 C 0.6983(3) 0.5601(4) 0.7302(9) 0.0577 1.0000 Uani D U . . . .
C2 C 0.7415(3) 0.5580(4) 0.8338(10) 0.0548 1.0000 Uani D U . . . .
O1 O 0.7963(3) 0.5913(3) 0.8189(8) 0.0551 1.0000 Uani D U . . . .
C1 C 0.7210(5) 0.5124(5) 0.9740(14) 0.0808 1.0000 Uani D U . . . .
H61 H 0.7144 0.6236 0.2501 0.0704 1.0000 Uiso R . . . . .
H71 H 0.6412 0.5911 0.0429 0.0709 1.0000 Uiso R . . . . .
H91 H 0.5211 0.4900 0.3793 0.0644 1.0000 Uiso R . . . . .
H81 H 0.5896 0.5218 0.5979 0.0607 1.0000 Uiso R . . . . .
H31 H 0.6582 0.5380 0.7673 0.0690 1.0000 Uiso R . . . . .
H11 H 0.7555 0.5159 1.0357 0.0978 1.0000 Uiso R . . . . .
H12 H 0.6957 0.5187 1.0547 0.0978 1.0000 Uiso R . . . . .
H13 H 0.6984 0.4727 0.9231 0.0978 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.08023(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 . N1 9_655 2.227(6) yes
Cu1 . N1 10_555 2.227(6) yes
Cu1 . O1 6_666 2.068(6) yes
Cu1 . O2 6_666 1.966(5) yes
Cu1 . O2 . 1.966(5) yes
Cu1 . O1 . 2.068(6) yes
O2 . C4 . 1.271(6) yes
C4 . C5 . 1.504(7) yes
C4 . C3 . 1.389(7) yes
C5 . C6 . 1.388(7) yes
C5 . C8 . 1.377(7) yes
C6 . C7 . 1.377(7) yes
C6 . H61 . 0.950 no
C7 . N1 . 1.326(7) yes
C7 . H71 . 0.950 no
N1 . C9 . 1.338(7) yes
C9 . C8 . 1.369(7) yes
C9 . H91 . 0.950 no
C8 . H81 . 0.950 no
C3 . C2 . 1.404(7) yes
C3 . H31 . 0.950 no
C2 . O1 . 1.249(7) yes
C2 . C1 . 1.497(8) yes
C1 . H11 . 0.980 no
C1 . H12 . 0.980 no
C1 . H13 . 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
N1 9_655 Cu1 . N1 10_555 179.995 yes
N1 9_655 Cu1 . O1 6_666 93.7(3) yes
N1 10_555 Cu1 . O1 6_666 86.3(3) yes
N1 9_655 Cu1 . O2 6_666 90.2(2) yes
N1 10_555 Cu1 . O2 6_666 89.8(2) yes
O1 6_666 Cu1 . O2 6_666 90.5(2) yes
N1 9_655 Cu1 . O2 . 89.8(2) yes
N1 10_555 Cu1 . O2 . 90.2(2) yes
O1 6_666 Cu1 . O2 . 89.5(2) yes
O2 6_666 Cu1 . O2 . 179.994 yes
N1 9_655 Cu1 . O1 . 86.3(3) yes
N1 10_555 Cu1 . O1 . 93.7(3) yes
O1 6_666 Cu1 . O1 . 179.994 yes
O2 6_666 Cu1 . O1 . 89.5(2) yes
O2 . Cu1 . O1 . 90.5(2) yes
Cu1 . O2 . C4 . 125.0(4) yes
O2 . C4 . C5 . 114.7(4) yes
O2 . C4 . C3 . 125.7(5) yes
C5 . C4 . C3 . 119.5(4) yes
C4 . C5 . C6 . 119.6(4) yes
C4 . C5 . C8 . 123.5(4) yes
C6 . C5 . C8 . 116.8(4) yes
C5 . C6 . C7 . 120.0(5) yes
C5 . C6 . H61 . 120.0 no
C7 . C6 . H61 . 120.0 no
C6 . C7 . N1 . 123.2(5) yes
C6 . C7 . H71 . 118.4 no
N1 . C7 . H71 . 118.4 no
Cu1 16_545 N1 . C7 . 126.5(4) yes
Cu1 16_545 N1 . C9 . 117.4(4) yes
C7 . N1 . C9 . 116.2(5) yes
N1 . C9 . C8 . 124.5(5) yes
N1 . C9 . H91 . 117.8 no
C8 . C9 . H91 . 117.8 no
C5 . C8 . C9 . 119.2(5) yes
C5 . C8 . H81 . 120.4 no
C9 . C8 . H81 . 120.4 no
C4 . C3 . C2 . 125.0(5) yes
C4 . C3 . H31 . 117.5 no
C2 . C3 . H31 . 117.5 no
C3 . C2 . O1 . 125.3(5) yes
C3 . C2 . C1 . 118.1(5) yes
O1 . C2 . C1 . 116.6(6) yes
C2 . O1 . Cu1 . 122.7(4) yes
C2 . C1 . H11 . 109.5 no
C2 . C1 . H12 . 109.5 no
H11 . C1 . H12 . 109.5 no
C2 . C1 . H13 . 109.3 no
H11 . C1 . H13 . 109.5 no
H12 . C1 . H13 . 109.5 no



# 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
-16 24 2 x .
-11 18 1 x .
-14 22 0 x .
-5 3 1 x .
-11 19 0 x .
8 13 1 x .
-11 18 4 x .
-7 11 0 x .
-3 6 0 x .
-1 6 2 x .
-1 3 2 x .
-1 3 2 x .
-10 18 2 x .
-10 17 0 x .
-1 9 2 x .
3 3 3 x .
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_MeOH_052_Syn
_database_code_depnum_ccdc_archive 'CCDC 1564954'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2020-06-09 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_audit_creation_date             2016-06-08
_audit_creation_method           CRYSTALS_ver_14.61_build_5965

_oxford_structure_analysis_title 'late01_0m_a.res in R-3'
_chemical_name_systematic        ?
_chemical_melting_point          ?

#end of refcif 
_cell_length_a                   26.453(2)
_cell_length_b                   26.453(2)
_cell_length_c                   7.7499(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4696.5(8)

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_space_group_name_Hall  '-R 3  '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3

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            9

# Given Formula = C18 H18 Cu1 N2 O4 
# Dc =      1.24 Fooo =   1809.00 Mu =     10.67 M =    389.90
# Found Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.23 FOOO =   1791.00 Mu =     10.67 M =    387.88

_chemical_formula_sum            'C18 H16 Cu1 N2 O4'
_chemical_formula_moiety         'C18 H16 Cu1 N2 O4'
_chemical_compound_source        ?
_chemical_formula_weight         387.88


_cell_measurement_reflns_used    3708
_cell_measurement_theta_min      2
_cell_measurement_theta_max      18
_cell_measurement_temperature    293

_exptl_crystal_description       green
_exptl_crystal_colour            block
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1791
_exptl_absorpt_coefficient_mu    1.067

# Sheldrick geometric approximatio 0.81 0.90 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_T_max  0.90
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_device       Serial
_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       'USER DEFINED DATA COLLECTION'
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_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_ambient_pressure         520000
_diffrn_reflns_number            6339
_reflns_number_total             1724
_diffrn_reflns_av_R_equivalents  0.063
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 1724 
# Theoretical number of reflections is about 4267 


_diffrn_reflns_theta_min         1.540
_diffrn_reflns_theta_max         26.368
_diffrn_measured_fraction_theta_max 0.804

_diffrn_reflns_theta_full        25.840
_diffrn_measured_fraction_theta_full 0.807


_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_reflns_limit_h_min              -32
_reflns_limit_h_max              13
_reflns_limit_k_min              0
_reflns_limit_k_max              32
_reflns_limit_l_min              0
_reflns_limit_l_max              9

_oxford_diffrn_Wilson_B_factor   1.56
_oxford_diffrn_Wilson_scale      302.55

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.78
_refine_diff_density_max         0.80


# 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>-3.0\s(I)
_refine_ls_number_reflns         1710
_refine_ls_number_restraints     126
_refine_ls_number_parameters     115
_oxford_refine_ls_R_factor_ref   0.0953
_refine_ls_wR_factor_ref         0.1655
_refine_ls_goodness_of_fit_ref   1.0712
_refine_ls_shift/su_max          0.0001273
_refine_ls_shift/su_mean         0.0000189


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1711
_refine_ls_R_factor_all          0.0955
_refine_ls_wR_factor_all         0.1662

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                1226
_refine_ls_R_factor_gt           0.0669
_refine_ls_wR_factor_gt          0.1275

# 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, 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: 
 63.7 77.2 27.1 
;

# 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 0.8333 0.6667 0.6667 0.0384 1.0000 Uani S . . . . .
O2 O 0.76188(17) 0.63527(18) 0.5281(5) 0.0434 1.0000 Uani D U . . . .
C4 C 0.7126(2) 0.5931(3) 0.5750(6) 0.0449 1.0000 Uani D U . . . .
C5 C 0.6639(2) 0.5762(3) 0.4481(6) 0.0431 1.0000 Uani D U . . . .
C6 C 0.6772(2) 0.5958(3) 0.2779(7) 0.0594 1.0000 Uani D U . . . .
C7 C 0.6333(3) 0.5764(3) 0.1574(7) 0.0613 1.0000 Uani D U . . . .
N1 N 0.5775(2) 0.5393(3) 0.1930(6) 0.0539 1.0000 Uani D U . . . .
C9 C 0.5649(2) 0.5214(3) 0.3568(6) 0.0492 1.0000 Uani D U . . . .
C8 C 0.6053(2) 0.5387(3) 0.4870(6) 0.0463 1.0000 Uani D U . . . .
C3 C 0.7019(3) 0.5601(3) 0.7235(7) 0.0617 1.0000 Uani D U . . . .
C2 C 0.7451(2) 0.5604(3) 0.8312(7) 0.0554 1.0000 Uani D U . . . .
O1 O 0.79879(19) 0.5955(2) 0.8178(5) 0.0520 1.0000 Uani D U . . . .
C1 C 0.7264(4) 0.5152(4) 0.9693(11) 0.0907 1.0000 Uani D U . . . .
H61 H 0.7164 0.6224 0.2457 0.0715 1.0000 Uiso R . . . . .
H71 H 0.6434 0.5901 0.0422 0.0733 1.0000 Uiso R . . . . .
H91 H 0.5252 0.4950 0.3848 0.0588 1.0000 Uiso R . . . . .
H81 H 0.5936 0.5252 0.6016 0.0556 1.0000 Uiso R . . . . .
H31 H 0.6623 0.5354 0.7558 0.0741 1.0000 Uiso R . . . . .
H11 H 0.7607 0.5206 1.0332 0.1103 1.0000 Uiso R . . . . .
H12 H 0.6997 0.5191 1.0485 0.1103 1.0000 Uiso R . . . . .
H13 H 0.7065 0.4762 0.9171 0.1103 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.4443(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 . N1 10_555 2.322(5) yes
Cu1 . N1 9_655 2.322(5) yes
Cu1 . O1 6_666 2.007(5) yes
Cu1 . O2 6_666 1.961(4) yes
Cu1 . O2 . 1.961(4) yes
Cu1 . O1 . 2.007(5) yes
O2 . C4 . 1.274(5) yes
C4 . C5 . 1.500(6) yes
C4 . C3 . 1.386(6) yes
C5 . C6 . 1.397(6) yes
C5 . C8 . 1.392(6) yes
C6 . C7 . 1.374(6) yes
C6 . H61 . 0.950 no
C7 . N1 . 1.330(6) yes
C7 . H71 . 0.950 no
N1 . C9 . 1.337(6) yes
C9 . C8 . 1.373(6) yes
C9 . H91 . 0.950 no
C8 . H81 . 0.950 no
C3 . C2 . 1.412(6) yes
C3 . H31 . 0.950 no
C2 . O1 . 1.254(6) yes
C2 . C1 . 1.494(7) yes
C1 . H11 . 0.980 no
C1 . H12 . 0.980 no
C1 . H13 . 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
N1 10_555 Cu1 . N1 9_655 179.995 yes
N1 10_555 Cu1 . O1 6_666 86.5(2) yes
N1 9_655 Cu1 . O1 6_666 93.5(2) yes
N1 10_555 Cu1 . O2 6_666 89.46(18) yes
N1 9_655 Cu1 . O2 6_666 90.54(18) yes
O1 6_666 Cu1 . O2 6_666 91.82(17) yes
N1 10_555 Cu1 . O2 . 90.54(18) yes
N1 9_655 Cu1 . O2 . 89.46(18) yes
O1 6_666 Cu1 . O2 . 88.18(17) yes
O2 6_666 Cu1 . O2 . 179.994 yes
N1 10_555 Cu1 . O1 . 93.5(2) yes
N1 9_655 Cu1 . O1 . 86.5(2) yes
O1 6_666 Cu1 . O1 . 179.994 yes
O2 6_666 Cu1 . O1 . 88.18(17) yes
O2 . Cu1 . O1 . 91.82(17) yes
Cu1 . O2 . C4 . 124.3(3) yes
O2 . C4 . C5 . 115.2(4) yes
O2 . C4 . C3 . 125.8(4) yes
C5 . C4 . C3 . 118.8(4) yes
C4 . C5 . C6 . 119.3(4) yes
C4 . C5 . C8 . 123.7(4) yes
C6 . C5 . C8 . 117.0(4) yes
C5 . C6 . C7 . 119.6(4) yes
C5 . C6 . H61 . 120.2 no
C7 . C6 . H61 . 120.2 no
C6 . C7 . N1 . 123.6(5) yes
C6 . C7 . H71 . 118.2 no
N1 . C7 . H71 . 118.2 no
Cu1 16_545 N1 . C7 . 127.0(3) yes
Cu1 16_545 N1 . C9 . 116.4(4) yes
C7 . N1 . C9 . 116.6(4) yes
N1 . C9 . C8 . 124.4(4) yes
N1 . C9 . H91 . 117.8 no
C8 . C9 . H91 . 117.8 no
C5 . C8 . C9 . 118.9(4) yes
C5 . C8 . H81 . 120.6 no
C9 . C8 . H81 . 120.6 no
C4 . C3 . C2 . 125.3(4) yes
C4 . C3 . H31 . 117.4 no
C2 . C3 . H31 . 117.3 no
C3 . C2 . O1 . 124.7(4) yes
C3 . C2 . C1 . 118.5(5) yes
O1 . C2 . C1 . 116.8(5) yes
C2 . O1 . Cu1 . 123.9(4) yes
C2 . C1 . H11 . 109.5 no
C2 . C1 . H12 . 109.3 no
H11 . C1 . H12 . 109.5 no
C2 . C1 . H13 . 109.6 no
H11 . C1 . H13 . 109.5 no
H12 . C1 . H13 . 109.5 no



# 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
-8 17 5 x .
-2 6 4 x .
-3 6 0 x .
-9 19 5 x .
-16 24 2 x .
-11 18 1 x .
-14 22 0 x .
-13 21 2 x .
10 16 3 x .
-11 8 5 x .
8 9 5 x .
-3 5 1 x .
2 4 4 x .
-8 11 5 x .
2 3 2 x .
-10 9 2 x .
-4 9 2 x .
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_MeOH_157_Syn
_database_code_depnum_ccdc_archive 'CCDC 1564956'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2020-06-09 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_audit_creation_date             2016-06-08
_audit_creation_method           CRYSTALS_ver_14.61_build_5965

_oxford_structure_analysis_title 'LATE03_0m in R-3'
_chemical_name_systematic        ?
_chemical_melting_point          ?

#end of refcif 
_cell_length_a                   25.4451(17)
_cell_length_b                   25.4451(17)
_cell_length_c                   7.7312(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4335.0(6)

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3

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            9

# Given Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.34 Fooo =   1791.00 Mu =     11.56 M =    387.88
# Found Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.34 FOOO =   1791.00 Mu =     11.56 M =    387.88

_chemical_formula_sum            'C18 H16 Cu1 N2 O4'
_chemical_formula_moiety         'C18 H16 Cu1 N2 O4'
_chemical_compound_source        ?
_chemical_formula_weight         387.88


_cell_measurement_reflns_used    4443
_cell_measurement_theta_min      2
_cell_measurement_theta_max      18
_cell_measurement_temperature    293

_exptl_crystal_description       green
_exptl_crystal_colour            block
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1791
_exptl_absorpt_coefficient_mu    1.156

# Sheldrick geometric approximatio 0.79 0.89 
_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  0.89
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_device       Serial
_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       'USER DEFINED DATA COLLECTION'
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_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_ambient_pressure         1570000
_diffrn_reflns_number            7358
_reflns_number_total             1669
_diffrn_reflns_av_R_equivalents  0.059
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 1669 
# Theoretical number of reflections is about 4084 


_diffrn_reflns_theta_min         2.773
_diffrn_reflns_theta_max         26.714
_diffrn_measured_fraction_theta_max 0.814

_diffrn_reflns_theta_full        26.714
_diffrn_measured_fraction_theta_full 0.814


_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_reflns_limit_h_min              -31
_reflns_limit_h_max              15
_reflns_limit_k_min              0
_reflns_limit_k_max              32
_reflns_limit_l_min              0
_reflns_limit_l_max              9

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.52
_refine_diff_density_max         0.58


# 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>-3.0\s(I)
_refine_ls_number_reflns         1652
_refine_ls_number_restraints     126
_refine_ls_number_parameters     115
_oxford_refine_ls_R_factor_ref   0.0809
_refine_ls_wR_factor_ref         0.2098
_refine_ls_goodness_of_fit_ref   0.9937
_refine_ls_shift/su_max          0.0001420
_refine_ls_shift/su_mean         0.0000170


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1652
_refine_ls_R_factor_all          0.0809
_refine_ls_wR_factor_all         0.2098

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                1266
_refine_ls_R_factor_gt           0.0608
_refine_ls_wR_factor_gt          0.1666

# 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, 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: 
 16.3 23.0 10.6 2.48 
;

# 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 0.8333 0.6667 0.6667 0.0308 1.0000 Uani S . . . . .
O2 O 0.75722(16) 0.63441(18) 0.5353(5) 0.0386 1.0000 Uani D U . . . .
C4 C 0.70569(19) 0.5915(2) 0.5822(6) 0.0353 1.0000 Uani D U . . . .
C5 C 0.65652(19) 0.5736(2) 0.4500(5) 0.0339 1.0000 Uani D U . . . .
C6 C 0.6709(2) 0.5969(3) 0.2841(7) 0.0468 1.0000 Uani D U . . . .
C7 C 0.6271(2) 0.5762(3) 0.1577(7) 0.0490 1.0000 Uani D U . . . .
N1 N 0.5698(2) 0.5336(2) 0.1864(5) 0.0391 1.0000 Uani D U . . . .
C9 C 0.5556(2) 0.5128(3) 0.3480(6) 0.0458 1.0000 Uani D U . . . .
C8 C 0.5962(2) 0.5302(3) 0.4812(6) 0.0430 1.0000 Uani D U . . . .
C3 C 0.6927(2) 0.5580(3) 0.7332(7) 0.0466 1.0000 Uani D U . . . .
C2 C 0.7358(2) 0.5546(3) 0.8414(7) 0.0452 1.0000 Uani D U . . . .
O1 O 0.79217(19) 0.5854(2) 0.8229(5) 0.0476 1.0000 Uani D U . . . .
C1 C 0.7127(4) 0.5065(4) 0.9787(12) 0.0846 1.0000 Uani D U . . . .
H61 H 0.7113 0.6275 0.2577 0.0567 1.0000 Uiso R . . . . .
H71 H 0.6383 0.5927 0.0446 0.0590 1.0000 Uiso R . . . . .
H91 H 0.5144 0.4839 0.3720 0.0552 1.0000 Uiso R . . . . .
H81 H 0.5835 0.5129 0.5929 0.0521 1.0000 Uiso R . . . . .
H31 H 0.6514 0.5356 0.7676 0.0562 1.0000 Uiso R . . . . .
H11 H 0.7469 0.5090 1.0436 0.1021 1.0000 Uiso R . . . . .
H12 H 0.6863 0.5130 1.0576 0.1021 1.0000 Uiso R . . . . .
H13 H 0.6895 0.4664 0.9252 0.1021 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.1581(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 6_666 2.161(4) yes
Cu1 . N1 9_655 2.108(4) yes
Cu1 . N1 10_555 2.108(4) yes
Cu1 . O2 6_666 1.966(4) yes
Cu1 . O2 . 1.966(4) yes
Cu1 . O1 . 2.161(4) yes
O2 . C4 . 1.269(5) yes
C4 . C5 . 1.499(5) yes
C4 . C3 . 1.385(6) yes
C5 . C6 . 1.384(6) yes
C5 . C8 . 1.393(6) yes
C6 . C7 . 1.374(6) yes
C6 . H61 . 0.950 no
C7 . N1 . 1.330(6) yes
C7 . H71 . 0.950 no
N1 . C9 . 1.334(5) yes
C9 . C8 . 1.366(6) yes
C9 . H91 . 0.950 no
C8 . H81 . 0.950 no
C3 . C2 . 1.415(6) yes
C3 . H31 . 0.950 no
C2 . O1 . 1.252(6) yes
C2 . C1 . 1.500(7) yes
C1 . H11 . 0.980 no
C1 . H12 . 0.980 no
C1 . H13 . 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
O1 6_666 Cu1 . N1 9_655 94.13(17) yes
O1 6_666 Cu1 . N1 10_555 85.87(17) yes
N1 9_655 Cu1 . N1 10_555 179.995 yes
O1 6_666 Cu1 . O2 6_666 89.09(15) yes
N1 9_655 Cu1 . O2 6_666 89.70(16) yes
N1 10_555 Cu1 . O2 6_666 90.30(16) yes
O1 6_666 Cu1 . O2 . 90.91(15) yes
N1 9_655 Cu1 . O2 . 90.30(16) yes
N1 10_555 Cu1 . O2 . 89.70(16) yes
O2 6_666 Cu1 . O2 . 179.994 yes
O1 6_666 Cu1 . O1 . 179.995 yes
N1 9_655 Cu1 . O1 . 85.87(17) yes
N1 10_555 Cu1 . O1 . 94.13(17) yes
O2 6_666 Cu1 . O1 . 90.91(15) yes
O2 . Cu1 . O1 . 89.09(15) yes
Cu1 . O2 . C4 . 126.2(3) yes
O2 . C4 . C5 . 114.4(4) yes
O2 . C4 . C3 . 126.5(4) yes
C5 . C4 . C3 . 118.8(4) yes
C4 . C5 . C6 . 120.0(3) yes
C4 . C5 . C8 . 123.0(3) yes
C6 . C5 . C8 . 116.8(4) yes
C5 . C6 . C7 . 120.3(4) yes
C5 . C6 . H61 . 119.8 no
C7 . C6 . H61 . 119.9 no
C6 . C7 . N1 . 122.9(4) yes
C6 . C7 . H71 . 118.6 no
N1 . C7 . H71 . 118.6 no
C7 . N1 . Cu1 16_545 125.1(3) yes
C7 . N1 . C9 . 116.7(4) yes
Cu1 16_545 N1 . C9 . 118.2(3) yes
N1 . C9 . C8 . 124.5(4) yes
N1 . C9 . H91 . 117.8 no
C8 . C9 . H91 . 117.7 no
C5 . C8 . C9 . 118.8(4) yes
C5 . C8 . H81 . 120.6 no
C9 . C8 . H81 . 120.6 no
C4 . C3 . C2 . 125.7(4) yes
C4 . C3 . H31 . 117.2 no
C2 . C3 . H31 . 117.1 no
C3 . C2 . O1 . 125.0(4) yes
C3 . C2 . C1 . 118.0(4) yes
O1 . C2 . C1 . 116.8(5) yes
Cu1 . O1 . C2 . 121.2(3) yes
C2 . C1 . H11 . 109.7 no
C2 . C1 . H12 . 109.0 no
H11 . C1 . H12 . 109.5 no
C2 . C1 . H13 . 109.7 no
H11 . C1 . H13 . 109.5 no
H12 . C1 . H13 . 109.5 no



# 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
-7 7 1 x .
-7 7 1 x .
-3 6 0 x .
-14 22 0 x .
-11 18 1 x .
-18 26 1 x .
8 12 2 x .
10 18 4 x .
-17 25 3 x .
-18 26 4 x .
-20 28 3 x .
-11 19 0 x .
-5 18 4 x .
-8 17 5 x .
2 4 4 x .
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_MeOH_215_Syn
_database_code_depnum_ccdc_archive 'CCDC 1564957'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2020-06-09 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_audit_creation_date             2016-06-08
_audit_creation_method           CRYSTALS_ver_14.61_build_5965

_oxford_structure_analysis_title 'LATE04_0m in R-3'
_chemical_name_systematic        ?
_chemical_melting_point          ?

#end of refcif 
_cell_length_a                   25.1855(18)
_cell_length_b                   25.1855(18)
_cell_length_c                   7.7300(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4246.3(6)

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3

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            9

# Given Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.37 Fooo =   1791.00 Mu =     11.80 M =    387.88
# Found Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.37 FOOO =   1791.00 Mu =     11.80 M =    387.88

_chemical_formula_sum            'C18 H16 Cu1 N2 O4'
_chemical_formula_moiety         'C18 H16 Cu1 N2 O4'
_chemical_compound_source        ?
_chemical_formula_weight         387.88


_cell_measurement_reflns_used    1666
_cell_measurement_theta_min      2
_cell_measurement_theta_max      18
_cell_measurement_temperature    293

_exptl_crystal_description       green
_exptl_crystal_colour            block
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1791
_exptl_absorpt_coefficient_mu    1.180

# Sheldrick geometric approximatio 0.79 0.89 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_T_max  0.89
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_device       Serial
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           '  ?   '
_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        '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_ambient_pressure         2150000
_diffrn_reflns_number            6405
_reflns_number_total             1700
_diffrn_reflns_av_R_equivalents  0.088
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 1700 
# Theoretical number of reflections is about 3888 


_diffrn_reflns_theta_min         1.105
_diffrn_reflns_theta_max         17.724
_diffrn_measured_fraction_theta_max 0.873

_diffrn_reflns_theta_full        13.825
_diffrn_measured_fraction_theta_full 0.892


_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_reflns_limit_h_min              -31
_reflns_limit_h_max              15
_reflns_limit_k_min              0
_reflns_limit_k_max              31
_reflns_limit_l_min              0
_reflns_limit_l_max              9

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.27
_refine_diff_density_max         1.31


# 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>-3.0\s(I)
_refine_ls_number_reflns         1694
_refine_ls_number_restraints     126
_refine_ls_number_parameters     115
_oxford_refine_ls_R_factor_ref   0.1126
_refine_ls_wR_factor_ref         0.1913
_refine_ls_goodness_of_fit_ref   1.0343
_refine_ls_shift/su_max          0.0001535
_refine_ls_shift/su_mean         0.0000163


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1694
_refine_ls_R_factor_all          0.1126
_refine_ls_wR_factor_all         0.1913

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                1021
_refine_ls_R_factor_gt           0.0631
_refine_ls_wR_factor_gt          0.1298

# 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, 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: 
 7.51 8.72 2.44 
;

# 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 0.8333 0.6667 0.6667 0.0327 1.0000 Uani S . . . . .
O2 O 0.7568(2) 0.6347(2) 0.5372(6) 0.0365 1.0000 Uani D U . . . .
C4 C 0.7043(2) 0.5910(3) 0.5850(7) 0.0331 1.0000 Uani D U . . . .
C5 C 0.6548(2) 0.5733(3) 0.4525(7) 0.0330 1.0000 Uani D U . . . .
C6 C 0.6697(3) 0.5985(4) 0.2879(8) 0.0459 1.0000 Uani D U . . . .
C7 C 0.6260(3) 0.5767(4) 0.1597(8) 0.0488 1.0000 Uani D U . . . .
N1 N 0.5686(3) 0.5328(3) 0.1856(6) 0.0365 1.0000 Uani D U . . . .
C9 C 0.5540(3) 0.5104(4) 0.3462(8) 0.0451 1.0000 Uani D U . . . .
C8 C 0.5946(3) 0.5283(4) 0.4805(7) 0.0428 1.0000 Uani D U . . . .
C3 C 0.6913(3) 0.5587(4) 0.7376(8) 0.0457 1.0000 Uani D U . . . .
C2 C 0.7337(3) 0.5535(4) 0.8452(8) 0.0461 1.0000 Uani D U . . . .
O1 O 0.7903(2) 0.5826(3) 0.8248(7) 0.0463 1.0000 Uani D U . . . .
C1 C 0.7088(5) 0.5067(5) 0.9877(14) 0.0900 1.0000 Uani D U . . . .
H61 H 0.7100 0.6309 0.2638 0.0551 1.0000 Uiso R . . . . .
H71 H 0.6376 0.5938 0.0472 0.0584 1.0000 Uiso R . . . . .
H91 H 0.5126 0.4801 0.3685 0.0542 1.0000 Uiso R . . . . .
H81 H 0.5817 0.5101 0.5915 0.0514 1.0000 Uiso R . . . . .
H31 H 0.6497 0.5380 0.7742 0.0548 1.0000 Uiso R . . . . .
H11 H 0.7428 0.5078 1.0522 0.1087 1.0000 Uiso R . . . . .
H12 H 0.6838 0.5159 1.0661 0.1087 1.0000 Uiso R . . . . .
H13 H 0.6834 0.4658 0.9375 0.1087 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.09006(7)
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 6_666 2.204(6) yes
Cu1 . N1 9_655 2.073(5) yes
Cu1 . N1 10_555 2.073(5) yes
Cu1 . O2 6_666 1.952(5) yes
Cu1 . O2 . 1.952(5) yes
Cu1 . O1 . 2.204(6) yes
O2 . C4 . 1.282(6) yes
C4 . C5 . 1.498(6) yes
C4 . C3 . 1.376(6) yes
C5 . C6 . 1.388(6) yes
C5 . C8 . 1.382(7) yes
C6 . C7 . 1.374(7) yes
C6 . H61 . 0.950 no
C7 . N1 . 1.326(7) yes
C7 . H71 . 0.950 no
N1 . C9 . 1.337(6) yes
C9 . C8 . 1.367(7) yes
C9 . H91 . 0.950 no
C8 . H81 . 0.950 no
C3 . C2 . 1.409(7) yes
C3 . H31 . 0.950 no
C2 . O1 . 1.245(6) yes
C2 . C1 . 1.503(7) yes
C1 . H11 . 0.980 no
C1 . H12 . 0.980 no
C1 . H13 . 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
O1 6_666 Cu1 . N1 9_655 94.4(2) yes
O1 6_666 Cu1 . N1 10_555 85.6(2) yes
N1 9_655 Cu1 . N1 10_555 179.994 yes
O1 6_666 Cu1 . O2 6_666 88.7(2) yes
N1 9_655 Cu1 . O2 6_666 89.5(2) yes
N1 10_555 Cu1 . O2 6_666 90.5(2) yes
O1 6_666 Cu1 . O2 . 91.3(2) yes
N1 9_655 Cu1 . O2 . 90.5(2) yes
N1 10_555 Cu1 . O2 . 89.5(2) yes
O2 6_666 Cu1 . O2 . 179.994 yes
O1 6_666 Cu1 . O1 . 179.995 yes
N1 9_655 Cu1 . O1 . 85.6(2) yes
N1 10_555 Cu1 . O1 . 94.4(2) yes
O2 6_666 Cu1 . O1 . 91.3(2) yes
O2 . Cu1 . O1 . 88.7(2) yes
Cu1 . O2 . C4 . 126.1(4) yes
O2 . C4 . C5 . 114.0(4) yes
O2 . C4 . C3 . 126.3(5) yes
C5 . C4 . C3 . 119.6(4) yes
C4 . C5 . C6 . 119.7(4) yes
C4 . C5 . C8 . 123.0(4) yes
C6 . C5 . C8 . 117.0(4) yes
C5 . C6 . C7 . 119.9(5) yes
C5 . C6 . H61 . 120.1 no
C7 . C6 . H61 . 120.1 no
C6 . C7 . N1 . 123.2(5) yes
C6 . C7 . H71 . 118.4 no
N1 . C7 . H71 . 118.4 no
C7 . N1 . Cu1 16_545 124.9(4) yes
C7 . N1 . C9 . 116.5(5) yes
Cu1 16_545 N1 . C9 . 118.4(4) yes
N1 . C9 . C8 . 124.3(5) yes
N1 . C9 . H91 . 117.9 no
C8 . C9 . H91 . 117.8 no
C5 . C8 . C9 . 119.0(5) yes
C5 . C8 . H81 . 120.5 no
C9 . C8 . H81 . 120.5 no
C4 . C3 . C2 . 126.5(5) yes
C4 . C3 . H31 . 116.8 no
C2 . C3 . H31 . 116.8 no
C3 . C2 . O1 . 124.6(5) yes
C3 . C2 . C1 . 117.9(5) yes
O1 . C2 . C1 . 117.3(5) yes
Cu1 . O1 . C2 . 120.2(4) yes
C2 . C1 . H11 . 109.6 no
C2 . C1 . H12 . 109.5 no
H11 . C1 . H12 . 109.5 no
C2 . C1 . H13 . 109.3 no
H11 . C1 . H13 . 109.5 no
H12 . C1 . H13 . 109.5 no


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_MeOH_278_Syn
_database_code_depnum_ccdc_archive 'CCDC 1564958'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2020-06-09 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_audit_creation_date             2016-06-08
_audit_creation_method           CRYSTALS_ver_14.61_build_5965

_oxford_structure_analysis_title 'late05_0m_a.res in R-3'
_chemical_name_systematic        ?
_chemical_melting_point          ?

#end of refcif 
_cell_length_a                   24.8906(16)
_cell_length_b                   24.8906(16)
_cell_length_c                   7.7570(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4161.9(6)

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3

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            9

# Given Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.39 Fooo =   1791.00 Mu =     12.04 M =    387.88
# Found Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.39 FOOO =   1791.00 Mu =     12.04 M =    387.88

_chemical_formula_sum            'C18 H16 Cu1 N2 O4'
_chemical_formula_moiety         'C18 H16 Cu1 N2 O4'
_chemical_compound_source        ?
_chemical_formula_weight         387.88


_cell_measurement_reflns_used    3468
_cell_measurement_theta_min      2
_cell_measurement_theta_max      16
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1791
_exptl_absorpt_coefficient_mu    1.204

# Sheldrick geometric approximatio 0.79 0.89 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_T_max  0.89
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_device       Serial
_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       'USER DEFINED DATA COLLECTION'
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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      293
_diffrn_reflns_number            7979
_reflns_number_total             1623
_diffrn_reflns_av_R_equivalents  0.071
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 1623 
# Theoretical number of reflections is about 3776 


_diffrn_reflns_theta_min         2.791
_diffrn_reflns_theta_max         26.354
_diffrn_measured_fraction_theta_max 0.857

_diffrn_reflns_theta_full        26.354
_diffrn_measured_fraction_theta_full 0.857


_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_reflns_limit_h_min              -30
_reflns_limit_h_max              14
_reflns_limit_k_min              0
_reflns_limit_k_max              31
_reflns_limit_l_min              0
_reflns_limit_l_max              9

_oxford_diffrn_Wilson_B_factor   2.66
_oxford_diffrn_Wilson_scale      14.00

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.57
_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>-3.0\s(I)
_refine_ls_number_reflns         1599
_refine_ls_number_restraints     126
_refine_ls_number_parameters     115
_oxford_refine_ls_R_factor_ref   0.1135
_refine_ls_wR_factor_ref         0.1517
_refine_ls_goodness_of_fit_ref   1.0283
_refine_ls_shift/su_max          0.0000979
_refine_ls_shift/su_mean         0.0000113


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1600
_refine_ls_R_factor_all          0.1138
_refine_ls_wR_factor_all         0.1519

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                1146
_refine_ls_R_factor_gt           0.0802
_refine_ls_wR_factor_gt          0.1257

# 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, 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: 
 36.5 37.4 12.4 
;

# 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 0.8333 0.6667 0.6667 0.0454 1.0000 Uani S . . . . .
O2 O 0.7558(2) 0.6343(3) 0.5398(5) 0.0518 1.0000 Uani D U . . . .
C4 C 0.7029(3) 0.5909(3) 0.5882(7) 0.0453 1.0000 Uani D U . . . .
C5 C 0.6534(3) 0.5728(3) 0.4549(6) 0.0462 1.0000 Uani D U . . . .
C6 C 0.6696(3) 0.5997(4) 0.2921(8) 0.0573 1.0000 Uani D U . . . .
C7 C 0.6259(3) 0.5779(4) 0.1626(8) 0.0570 1.0000 Uani D U . . . .
N1 N 0.5679(3) 0.5321(3) 0.1858(6) 0.0493 1.0000 Uani D U . . . .
C9 C 0.5520(3) 0.5084(4) 0.3450(7) 0.0576 1.0000 Uani D U . . . .
C8 C 0.5933(3) 0.5266(4) 0.4792(7) 0.0543 1.0000 Uani D U . . . .
C3 C 0.6890(3) 0.5584(4) 0.7420(8) 0.0582 1.0000 Uani D U . . . .
C2 C 0.7318(3) 0.5537(4) 0.8492(8) 0.0570 1.0000 Uani D U . . . .
O1 O 0.7887(3) 0.5808(3) 0.8276(6) 0.0564 1.0000 Uani D U . . . .
C1 C 0.7077(5) 0.5089(5) 0.9977(12) 0.0986 1.0000 Uani D U . . . .
H61 H 0.7102 0.6330 0.2702 0.0663 1.0000 Uiso R . . . . .
H71 H 0.6380 0.5958 0.0511 0.0713 1.0000 Uiso R . . . . .
H91 H 0.5101 0.4778 0.3660 0.0693 1.0000 Uiso R . . . . .
H81 H 0.5806 0.5064 0.5877 0.0680 1.0000 Uiso R . . . . .
H31 H 0.6469 0.5378 0.7788 0.0706 1.0000 Uiso R . . . . .
H11 H 0.7427 0.5104 1.0601 0.1139 1.0000 Uiso R . . . . .
H12 H 0.6843 0.5207 1.0756 0.1139 1.0000 Uiso R . . . . .
H13 H 0.6805 0.4668 0.9549 0.1139 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.2821(6)
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 6_666 2.233(6) yes
Cu1 . N1 9_655 2.055(5) yes
Cu1 . N1 10_555 2.055(5) yes
Cu1 . O2 6_666 1.945(5) yes
Cu1 . O2 . 1.945(5) yes
Cu1 . O1 . 2.233(6) yes
O2 . C4 . 1.272(6) yes
C4 . C5 . 1.493(6) yes
C4 . C3 . 1.386(6) yes
C5 . C6 . 1.392(6) yes
C5 . C8 . 1.370(7) yes
C6 . C7 . 1.376(7) yes
C6 . H61 . 0.950 no
C7 . N1 . 1.331(7) yes
C7 . H71 . 0.950 no
N1 . C9 . 1.339(6) yes
C9 . C8 . 1.370(6) yes
C9 . H91 . 0.950 no
C8 . H81 . 0.950 no
C3 . C2 . 1.401(7) yes
C3 . H31 . 0.950 no
C2 . O1 . 1.239(6) yes
C2 . C1 . 1.504(7) yes
C1 . H11 . 0.980 no
C1 . H12 . 0.980 no
C1 . H13 . 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
O1 6_666 Cu1 . N1 9_655 95.3(2) yes
O1 6_666 Cu1 . N1 10_555 84.7(2) yes
N1 9_655 Cu1 . N1 10_555 179.994 yes
O1 6_666 Cu1 . O2 6_666 88.3(2) yes
N1 9_655 Cu1 . O2 6_666 89.1(2) yes
N1 10_555 Cu1 . O2 6_666 90.9(2) yes
O1 6_666 Cu1 . O2 . 91.7(2) yes
N1 9_655 Cu1 . O2 . 90.9(2) yes
N1 10_555 Cu1 . O2 . 89.1(2) yes
O2 6_666 Cu1 . O2 . 179.994 yes
O1 6_666 Cu1 . O1 . 179.995 yes
N1 9_655 Cu1 . O1 . 84.7(2) yes
N1 10_555 Cu1 . O1 . 95.3(2) yes
O2 6_666 Cu1 . O1 . 91.7(2) yes
O2 . Cu1 . O1 . 88.3(2) yes
Cu1 . O2 . C4 . 126.5(4) yes
O2 . C4 . C5 . 113.6(4) yes
O2 . C4 . C3 . 126.8(5) yes
C5 . C4 . C3 . 119.5(4) yes
C4 . C5 . C6 . 119.1(4) yes
C4 . C5 . C8 . 123.2(4) yes
C6 . C5 . C8 . 117.4(4) yes
C5 . C6 . C7 . 119.5(5) yes
C5 . C6 . H61 . 120.5 no
C7 . C6 . H61 . 120.1 no
C6 . C7 . N1 . 122.9(5) yes
C6 . C7 . H71 . 118.5 no
N1 . C7 . H71 . 118.6 no
C7 . N1 . Cu1 16_545 124.5(4) yes
C7 . N1 . C9 . 117.2(4) yes
Cu1 16_545 N1 . C9 . 118.1(4) yes
N1 . C9 . C8 . 123.2(5) yes
N1 . C9 . H91 . 118.3 no
C8 . C9 . H91 . 118.5 no
C9 . C8 . C5 . 119.8(4) yes
C9 . C8 . H81 . 120.1 no
C5 . C8 . H81 . 120.1 no
C4 . C3 . C2 . 125.5(5) yes
C4 . C3 . H31 . 117.4 no
C2 . C3 . H31 . 117.1 no
C3 . C2 . O1 . 125.8(5) yes
C3 . C2 . C1 . 118.5(5) yes
O1 . C2 . C1 . 115.5(5) yes
Cu1 . O1 . C2 . 118.8(4) yes
C2 . C1 . H11 . 109.4 no
C2 . C1 . H12 . 109.1 no
H11 . C1 . H12 . 109.5 no
C2 . C1 . H13 . 109.9 no
H11 . C1 . H13 . 109.5 no
H12 . C1 . H13 . 109.5 no



# 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
-16 24 2 x .
-11 18 1 x .
-14 22 0 x .
-5 3 1 x .
-11 19 0 x .
8 13 1 x .
-11 18 4 x .
-7 11 0 x .
-3 6 0 x .
-1 6 2 x .
-1 3 2 x .
-1 3 2 x .
-10 18 2 x .
-10 17 0 x .
-1 9 2 x .
3 3 3 x .
-18 26 1 x .
8 12 2 x .
-5 4 3 x .
-10 19 1 x .
-13 14 0 x .
-1 14 0 x .
-2 19 0 x .
-9 14 4 x .
-7 9 2 x .
-11 7 6 x .
-10 20 0 x .
-2 4 3 x .
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_FC70_000_Lab
_database_code_depnum_ccdc_archive 'CCDC 1564960'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2020-06-09 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_audit_creation_date             2016-06-08
_audit_creation_method           CRYSTALS_ver_14.61_build_5965

_oxford_structure_analysis_title 'st5049_0m_a.res in R-3'
_chemical_name_systematic        ?
_chemical_melting_point          ?

#end of refcif 
_cell_length_a                   26.594(3)
_cell_length_b                   26.594(3)
_cell_length_c                   7.7475(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4745.1(12)

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_space_group_name_Hall  '-R 3'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3

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            9

# Given Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.22 Fooo =   1791.00 Mu =     10.56 M =    387.88
# Found Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.22 FOOO =   1791.00 Mu =     10.56 M =    387.88

_chemical_formula_sum            'C18 H16 Cu1 N2 O4'
_chemical_formula_moiety         'C18 H16 Cu1 N2 O4'
_chemical_compound_source        ?
_chemical_formula_weight         387.88


_cell_measurement_reflns_used    2653
_cell_measurement_theta_min      3
_cell_measurement_theta_max      21
_cell_measurement_temperature    293

_exptl_crystal_description       green
_exptl_crystal_colour            block
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1791
_exptl_absorpt_coefficient_mu    1.056

# Sheldrick geometric approximatio 0.81 0.90 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_T_max  0.90
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_device       Serial
_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       'USER DEFINED DATA COLLECTION'
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_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            8742
_reflns_number_total             1737
_diffrn_reflns_av_R_equivalents  0.045
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 1737 
# Theoretical number of reflections is about 3472 


_diffrn_reflns_theta_min         2.653
_diffrn_reflns_theta_max         24.406
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        24.406
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_reflns_limit_h_min              -30
_reflns_limit_h_max              14
_reflns_limit_k_min              0
_reflns_limit_k_max              30
_reflns_limit_l_min              0
_reflns_limit_l_max              8

_oxford_diffrn_Wilson_B_factor   2.79
_oxford_diffrn_Wilson_scale      42.45

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.51
_refine_diff_density_max         0.65


# 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>-3.0\s(I)
_refine_ls_number_reflns         1730
_refine_ls_number_restraints     4
_refine_ls_number_parameters     115
_oxford_refine_ls_R_factor_ref   0.0609
_refine_ls_wR_factor_ref         0.0833
_refine_ls_goodness_of_fit_ref   0.9899
_refine_ls_shift/su_max          0.0002001
_refine_ls_shift/su_mean         0.0000242


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1730
_refine_ls_R_factor_all          0.0609
_refine_ls_wR_factor_all         0.0833

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                1338
_refine_ls_R_factor_gt           0.0452
_refine_ls_wR_factor_gt          0.0750

# 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, 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: 
 12.1 14.2 4.23 
;

# 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 0.8333 0.6667 0.6667 0.0401 1.0000 Uani S . . . . .
O2 O 0.76273(12) 0.63483(13) 0.5259(3) 0.0482 1.0000 Uani . . . . . .
C4 C 0.71445(18) 0.59029(19) 0.5666(5) 0.0467 1.0000 Uani . . . . . .
C5 C 0.66598(18) 0.57416(18) 0.4388(5) 0.0475 1.0000 Uani . . . . . .
C6 C 0.6782(2) 0.5927(2) 0.2691(6) 0.0683 1.0000 Uani . . . . . .
C7 C 0.6343(2) 0.5748(2) 0.1505(6) 0.0734 1.0000 Uani . . . . . .
N1 N 0.57893(16) 0.53904(17) 0.1886(4) 0.0559 1.0000 Uani . . . . . .
C9 C 0.56701(19) 0.5228(2) 0.3525(5) 0.0574 1.0000 Uani . . . . . .
C8 C 0.60827(19) 0.5386(2) 0.4795(5) 0.0550 1.0000 Uani . . . . . .
C3 C 0.7042(2) 0.5558(2) 0.7087(6) 0.0700 1.0000 Uani . . . . . .
C2 C 0.7460(2) 0.5588(2) 0.8246(6) 0.0604 1.0000 Uani D . . . . .
O1 O 0.79874(13) 0.59600(14) 0.8221(4) 0.0568 1.0000 Uani . . . . . .
C1 C 0.7264(2) 0.5118(3) 0.9635(7) 0.1013 1.0000 Uani D . . . . .
H61 H 0.7172 0.6180 0.2349 0.0813 1.0000 Uiso R . . . . .
H71 H 0.6441 0.5885 0.0353 0.0864 1.0000 Uiso R . . . . .
H91 H 0.5275 0.4986 0.3840 0.0669 1.0000 Uiso R . . . . .
H81 H 0.5970 0.5254 0.5946 0.0650 1.0000 Uiso R . . . . .
H31 H 0.6649 0.5273 0.7310 0.0824 1.0000 Uiso R . . . . .
H11 H 0.7509 0.5280 1.0656 0.1187 1.0000 Uiso DR . . . . .
H12 H 0.6860 0.4983 0.9945 0.1187 1.0000 Uiso DR . . . . .
H13 H 0.7298 0.4792 0.9208 0.1187 1.0000 Uiso DR . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.16740(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 . N1 9_655 2.332(3) yes
Cu1 . N1 10_555 2.332(3) yes
Cu1 . O1 6_666 2.025(3) yes
Cu1 . O2 6_666 1.960(3) yes
Cu1 . O2 . 1.960(3) yes
Cu1 . O1 . 2.025(3) yes
O2 . C4 . 1.277(5) yes
C4 . C5 . 1.507(5) yes
C4 . C3 . 1.371(6) yes
C5 . C6 . 1.385(6) yes
C5 . C8 . 1.377(6) yes
C6 . C7 . 1.369(6) yes
C6 . H61 . 0.950 no
C7 . N1 . 1.328(6) yes
C7 . H71 . 0.950 no
N1 . C9 . 1.328(5) yes
C9 . C8 . 1.374(6) yes
C9 . H91 . 0.950 no
C8 . H81 . 0.950 no
C3 . C2 . 1.400(6) yes
C3 . H31 . 0.950 no
C2 . O1 . 1.248(5) yes
C2 . C1 . 1.530(6) yes
C1 . H11 . 0.977 no
C1 . H12 . 0.977 no
C1 . H13 . 0.976 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
N1 9_655 Cu1 . N1 10_555 179.995 yes
N1 9_655 Cu1 . O1 6_666 92.83(13) yes
N1 10_555 Cu1 . O1 6_666 87.17(13) yes
N1 9_655 Cu1 . O2 6_666 90.17(12) yes
N1 10_555 Cu1 . O2 6_666 89.83(12) yes
O1 6_666 Cu1 . O2 6_666 92.15(12) yes
N1 9_655 Cu1 . O2 . 89.83(12) yes
N1 10_555 Cu1 . O2 . 90.17(12) yes
O1 6_666 Cu1 . O2 . 87.85(12) yes
O2 6_666 Cu1 . O2 . 179.994 yes
N1 9_655 Cu1 . O1 . 87.17(13) yes
N1 10_555 Cu1 . O1 . 92.83(13) yes
O1 6_666 Cu1 . O1 . 179.994 yes
O2 6_666 Cu1 . O1 . 87.85(12) yes
O2 . Cu1 . O1 . 92.15(12) yes
Cu1 . O2 . C4 . 124.4(3) yes
O2 . C4 . C5 . 115.0(4) yes
O2 . C4 . C3 . 126.2(4) yes
C5 . C4 . C3 . 118.8(4) yes
C4 . C5 . C6 . 120.5(4) yes
C4 . C5 . C8 . 123.1(4) yes
C6 . C5 . C8 . 116.4(4) yes
C5 . C6 . C7 . 120.4(4) yes
C5 . C6 . H61 . 119.7 no
C7 . C6 . H61 . 119.9 no
C6 . C7 . N1 . 123.2(4) yes
C6 . C7 . H71 . 118.3 no
N1 . C7 . H71 . 118.5 no
Cu1 16_545 N1 . C7 . 127.5(3) yes
Cu1 16_545 N1 . C9 . 116.0(3) yes
C7 . N1 . C9 . 116.4(4) yes
N1 . C9 . C8 . 124.1(4) yes
N1 . C9 . H91 . 118.0 no
C8 . C9 . H91 . 117.9 no
C5 . C8 . C9 . 119.4(4) yes
C5 . C8 . H81 . 120.3 no
C9 . C8 . H81 . 120.2 no
C4 . C3 . C2 . 126.1(4) yes
C4 . C3 . H31 . 116.9 no
C2 . C3 . H31 . 117.0 no
C3 . C2 . O1 . 125.6(4) yes
C3 . C2 . C1 . 117.8(4) yes
O1 . C2 . C1 . 116.6(4) yes
C2 . O1 . Cu1 . 123.6(3) yes
C2 . C1 . H11 . 109.2 no
C2 . C1 . H12 . 109.7 no
H11 . C1 . H12 . 109.4 no
C2 . C1 . H13 . 110.1 no
H11 . C1 . H13 . 109.1 no
H12 . C1 . H13 . 109.4 no


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_MeOH_334_Syn
_database_code_depnum_ccdc_archive 'CCDC 1564959'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2020-06-09 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_audit_creation_date             2016-06-10
_audit_creation_method           CRYSTALS_ver_14.61_build_5965

_oxford_structure_analysis_title 'LATE06_0m in R-3'
_chemical_name_systematic        ?
_chemical_melting_point          ?

#end of refcif 
_cell_length_a                   49.169(3)
_cell_length_b                   49.169(3)
_cell_length_c                   7.7897(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     16310(2)

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_space_group_name_Hall  '-R 3 '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3

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            18

# Given Formula = C53.33 H53.33 Cu5.33 N1.11 O26.67 
# Dc =      1.35 Fooo =   6742.00 Mu =     16.09 M =   1475.47
# Found Formula = C72 H64 Cu4 N8 O16 
# Dc =      1.42 FOOO =   7164.00 Mu =     12.29 M =   1551.53

_chemical_formula_sum            'C36 H32 Cu2 N4 O8'
_chemical_formula_moiety         'C36 H32 Cu2 N4 O8'
_chemical_compound_source        ?
_chemical_formula_weight         1551.53


_cell_measurement_reflns_used    5751
_cell_measurement_theta_min      2
_cell_measurement_theta_max      14
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             7164
_exptl_absorpt_coefficient_mu    1.229

# Sheldrick geometric approximatio 0.78 0.88 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_T_max  0.88
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_device       Serial
_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       'USER DEFINED DATA COLLECTION'
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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      293
_diffrn_reflns_number            10639
_reflns_number_total             2642
_diffrn_reflns_av_R_equivalents  0.111
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 2642 
# Theoretical number of reflections is about 7502 


_diffrn_reflns_theta_min         1.435
_diffrn_reflns_theta_max         20.731
_diffrn_measured_fraction_theta_max 0.705

_diffrn_reflns_theta_full        20.109
_diffrn_measured_fraction_theta_full 0.709


_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_reflns_limit_h_min              -47
_reflns_limit_h_max              20
_reflns_limit_k_min              0
_reflns_limit_k_max              48
_reflns_limit_l_min              0
_reflns_limit_l_max              7

_oxford_diffrn_Wilson_B_factor   2.47
_oxford_diffrn_Wilson_scale      1363.18

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -3.76
_refine_diff_density_max         2.96


# 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         1366
_refine_ls_number_restraints     236
_refine_ls_number_parameters     201
_oxford_refine_ls_R_factor_ref   0.1966
_refine_ls_wR_factor_ref         0.2282
_refine_ls_goodness_of_fit_ref   1.2142
_refine_ls_shift/su_max          0.0035154
_refine_ls_shift/su_mean         0.0001623


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        2575
_refine_ls_R_factor_all          0.2815
_refine_ls_wR_factor_all         0.4126

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                1366
_refine_ls_R_factor_gt           0.1966
_refine_ls_wR_factor_gt          0.2282

# 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: 
 1.87 1.41 0.956 
;

# 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 0.58084(11) 0.41298(11) -0.3231(6) 0.0286(17) 1.0000 Uiso . . . . . .
Cu2 Cu 0.41297(11) 0.32643(10) 0.3343(5) 0.0167(15) 1.0000 Uiso . . . . . .
C1 C 0.6481(7) 0.4043(8) 0.006(4) 0.045(4) 1.0000 Uiso D U . . . .
C2 C 0.6341(5) 0.4116(7) -0.150(3) 0.044(4) 1.0000 Uiso D U . . . .
C3 C 0.6542(5) 0.4371(6) -0.254(2) 0.044(4) 1.0000 Uiso D U . . . .
C4 C 0.6462(5) 0.4446(8) -0.408(3) 0.044(3) 1.0000 Uiso D U . . . .
C5 C 0.6707(4) 0.4594(2) -0.5468(18) 0.045(4) 1.0000 Uiso D U . . . .
C6 C 0.7005(4) 0.4636(2) -0.526(2) 0.045(4) 1.0000 Uiso D U . . . .
C7 C 0.7209(4) 0.4743(3) -0.662(3) 0.045(4) 1.0000 Uiso D U . . . .
C8 C 0.6838(5) 0.4767(2) -0.8353(19) 0.045(4) 1.0000 Uiso D U . . . .
C9 C 0.6625(4) 0.4660(2) -0.703(2) 0.045(4) 1.0000 Uiso D U . . . .
C11 C 0.5842(8) 0.5161(6) 0.687(3) 0.033(3) 1.0000 Uiso D U . . . .
C12 C 0.6028(8) 0.5288(5) 0.520(3) 0.032(3) 1.0000 Uiso D U . . . .
C13 C 0.6050(7) 0.5076(4) 0.408(3) 0.031(3) 1.0000 Uiso D U . . . .
C14 C 0.6221(6) 0.5154(4) 0.259(3) 0.030(3) 1.0000 Uiso D U . . . .
C15 C 0.6146(3) 0.4904(4) 0.1259(19) 0.030(3) 1.0000 Uiso D U . . . .
C16 C 0.5928(3) 0.4592(4) 0.156(2) 0.030(3) 1.0000 Uiso D U . . . .
C17 C 0.5841(3) 0.4382(4) 0.023(2) 0.031(3) 1.0000 Uiso D U . . . .
C18 C 0.6176(4) 0.4781(5) -0.160(2) 0.031(3) 1.0000 Uiso D U . . . .
C19 C 0.6267(4) 0.4996(5) -0.029(3) 0.030(3) 1.0000 Uiso D U . . . .
C21 C 0.4335(7) 0.4099(7) 0.663(3) 0.034(4) 1.0000 Uiso D U . . . .
C22 C 0.4198(6) 0.3842(6) 0.527(3) 0.034(3) 1.0000 Uiso D U . . . .
C23 C 0.3975(7) 0.3838(7) 0.413(3) 0.034(3) 1.0000 Uiso D U . . . .
C24 C 0.3871(7) 0.3667(5) 0.265(2) 0.034(3) 1.0000 Uiso D U . . . .
C25 C 0.3742(2) 0.3782(3) 0.1247(16) 0.034(3) 1.0000 Uiso D U . . . .
C26 C 0.3704(2) 0.4037(3) 0.1516(19) 0.034(3) 1.0000 Uiso D U . . . .
C27 C 0.3626(2) 0.4160(3) 0.015(2) 0.034(3) 1.0000 Uiso D U . . . .
C28 C 0.3619(2) 0.3789(4) -0.1674(18) 0.034(3) 1.0000 Uiso D U . . . .
C29 C 0.3698(2) 0.3655(3) -0.0360(19) 0.034(3) 1.0000 Uiso D U . . . .
C31 C 0.5162(7) 0.4196(8) -0.680(3) 0.040(4) 1.0000 Uiso D U . . . .
C32 C 0.5277(5) 0.4173(6) -0.501(2) 0.039(3) 1.0000 Uiso D U . . . .
C33 C 0.5069(4) 0.3924(6) -0.396(3) 0.038(3) 1.0000 Uiso D U . . . .
C34 C 0.5144(4) 0.3828(7) -0.247(3) 0.037(3) 1.0000 Uiso D U . . . .
C35 C 0.4891(4) 0.3654(2) -0.1151(17) 0.037(3) 1.0000 Uiso D U . . . .
C36 C 0.4973(4) 0.3597(2) 0.044(2) 0.037(3) 1.0000 Uiso D U . . . .
C37 C 0.4757(5) 0.3491(2) 0.1737(18) 0.037(3) 1.0000 Uiso D U . . . .
C38 C 0.4386(4) 0.3495(2) -0.004(2) 0.036(3) 1.0000 Uiso D U . . . .
C39 C 0.4594(4) 0.3603(2) -0.139(2) 0.037(3) 1.0000 Uiso D U . . . .
N1 N 0.7123(5) 0.4806(2) -0.813(2) 0.045(4) 1.0000 Uiso D U . . . .
N2 N 0.4468(5) 0.3441(2) 0.151(2) 0.036(3) 1.0000 Uiso D U . . . .
N3 N 0.3583(2) 0.4037(4) -0.142(2) 0.034(3) 1.0000 Uiso D U . . . .
N4 N 0.5967(4) 0.4480(5) -0.132(2) 0.031(3) 1.0000 Uiso D U . . . .
O1 O 0.6049(5) 0.3960(6) -0.164(3) 0.044(4) 1.0000 Uiso D U . . . .
O2 O 0.6191(5) 0.4402(7) -0.450(3) 0.044(4) 1.0000 Uiso D U . . . .
O11 O 0.6145(6) 0.5576(4) 0.495(3) 0.032(3) 1.0000 Uiso D U . . . .
O12 O 0.6430(5) 0.5429(4) 0.213(2) 0.029(3) 1.0000 Uiso D U . . . .
O21 O 0.4341(5) 0.3694(5) 0.505(3) 0.033(4) 1.0000 Uiso D U . . . .
O22 O 0.3917(6) 0.3443(5) 0.220(2) 0.034(3) 1.0000 Uiso D U . . . .
O31 O 0.5566(5) 0.4332(5) -0.478(3) 0.039(3) 1.0000 Uiso D U . . . .
O32 O 0.5419(4) 0.3902(6) -0.197(2) 0.037(3) 1.0000 Uiso D U . . . .
H11 H 0.6706 0.4171 0.0072 0.0473 1.0000 Uiso R . . . . .
H12 H 0.6396 0.4079 0.1091 0.0473 1.0000 Uiso R . . . . .
H13 H 0.6424 0.3826 0.0006 0.0473 1.0000 Uiso R . . . . .
H31 H 0.6755 0.4489 -0.2182 0.0473 1.0000 Uiso R . . . . .
H61 H 0.7070 0.4596 -0.4188 0.0465 1.0000 Uiso R . . . . .
H71 H 0.7416 0.4777 -0.6493 0.0465 1.0000 Uiso R . . . . .
H81 H 0.6779 0.4809 -0.9440 0.0467 1.0000 Uiso R . . . . .
H91 H 0.6419 0.4628 -0.7198 0.0467 1.0000 Uiso R . . . . .
H111 H 0.5737 0.4936 0.6889 0.0533 1.0000 Uiso R . . . . .
H112 H 0.5994 0.5244 0.7779 0.0533 1.0000 Uiso R . . . . .
H113 H 0.5690 0.5228 0.7019 0.0533 1.0000 Uiso R . . . . .
H131 H 0.5935 0.4861 0.4396 0.0538 1.0000 Uiso R . . . . .
H161 H 0.5839 0.4528 0.2672 0.0536 1.0000 Uiso R . . . . .
H171 H 0.5684 0.4170 0.0425 0.0534 1.0000 Uiso R . . . . .
H181 H 0.6263 0.4844 -0.2716 0.0537 1.0000 Uiso R . . . . .
H191 H 0.6426 0.5206 -0.0507 0.0536 1.0000 Uiso R . . . . .
H211 H 0.4221 0.4210 0.6616 0.0597 1.0000 Uiso R . . . . .
H212 H 0.4557 0.4247 0.6588 0.0597 1.0000 Uiso R . . . . .
H213 H 0.4287 0.3977 0.7660 0.0597 1.0000 Uiso R . . . . .
H231 H 0.3863 0.3936 0.4540 0.0598 1.0000 Uiso R . . . . .
H261 H 0.3735 0.4130 0.2618 0.0586 1.0000 Uiso R . . . . .
H271 H 0.3597 0.4335 0.0318 0.0584 1.0000 Uiso R . . . . .
H281 H 0.3587 0.3698 -0.2785 0.0582 1.0000 Uiso R . . . . .
H291 H 0.3725 0.3479 -0.0555 0.0585 1.0000 Uiso R . . . . .
H311 H 0.4937 0.4067 -0.6841 0.0579 1.0000 Uiso R . . . . .
H312 H 0.5221 0.4411 -0.7014 0.0579 1.0000 Uiso R . . . . .
H313 H 0.5254 0.4127 -0.7654 0.0579 1.0000 Uiso R . . . . .
H331 H 0.4860 0.3797 -0.4357 0.0581 1.0000 Uiso R . . . . .
H361 H 0.5177 0.3629 0.0650 0.0589 1.0000 Uiso R . . . . .
H371 H 0.4811 0.3448 0.2835 0.0592 1.0000 Uiso R . . . . .
H381 H 0.4180 0.3460 -0.0220 0.0590 1.0000 Uiso R . . . . .
H391 H 0.4534 0.3644 -0.2476 0.0589 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.0252(4)
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 . N1 16_543 2.111(17) yes
Cu1 . N4 . 2.108(17) yes
Cu1 . O1 . 2.15(2) yes
Cu1 . O2 . 1.94(2) yes
Cu1 . O31 . 2.25(2) yes
Cu1 . O32 . 1.935(19) yes
Cu2 . O11 16_545 2.31(2) yes
Cu2 . N3 15_555 2.080(15) yes
Cu2 . O12 16_545 1.838(18) yes
Cu2 . N2 . 2.029(16) yes
Cu2 . O21 . 2.26(2) yes
Cu2 . O22 . 1.893(18) yes
C1 . C2 . 1.526(9) yes
C1 . H11 . 0.960 no
C1 . H12 . 0.960 no
C1 . H13 . 0.960 no
C2 . C3 . 1.401(9) yes
C2 . O1 . 1.249(9) yes
C3 . C4 . 1.371(9) yes
C3 . H31 . 0.950 no
C4 . C5 . 1.509(9) yes
C4 . O2 . 1.281(9) yes
C5 . C6 . 1.382(9) yes
C5 . C9 . 1.372(9) yes
C6 . C7 . 1.373(9) yes
C6 . H61 . 0.950 no
C7 . N1 . 1.335(9) yes
C7 . H71 . 0.950 no
C8 . C9 . 1.375(9) yes
C8 . N1 . 1.328(9) yes
C8 . H81 . 0.950 no
C9 . H91 . 0.950 no
C11 . C12 . 1.529(9) yes
C11 . H111 . 0.960 no
C11 . H112 . 0.960 no
C11 . H113 . 0.960 no
C12 . C13 . 1.404(9) yes
C12 . O11 . 1.247(9) yes
C13 . C14 . 1.372(9) yes
C13 . H131 . 0.950 no
C14 . C15 . 1.507(9) yes
C14 . O12 . 1.276(9) yes
C15 . C16 . 1.383(9) yes
C15 . C19 . 1.32(3) yes
C16 . C17 . 1.370(9) yes
C16 . H161 . 0.950 no
C17 . N4 . 1.333(9) yes
C17 . H171 . 0.950 no
C18 . C19 . 1.370(9) yes
C18 . N4 . 1.334(9) yes
C18 . H181 . 0.950 no
C19 . H191 . 0.950 no
C21 . C22 . 1.526(9) yes
C21 . H211 . 0.960 no
C21 . H212 . 0.960 no
C21 . H213 . 0.960 no
C22 . C23 . 1.401(9) yes
C22 . O21 . 1.247(9) yes
C23 . C24 . 1.373(9) yes
C23 . H231 . 0.950 no
C24 . C25 . 1.507(9) yes
C24 . O22 . 1.277(9) yes
C25 . C26 . 1.374(9) yes
C25 . C29 . 1.366(9) yes
C26 . C27 . 1.370(9) yes
C26 . H261 . 0.950 no
C27 . N3 . 1.335(9) yes
C27 . H271 . 0.950 no
C28 . C29 . 1.372(9) yes
C28 . N3 . 1.333(9) yes
C28 . H281 . 0.950 no
C29 . H291 . 0.950 no
C31 . C32 . 1.528(9) yes
C31 . H311 . 0.960 no
C31 . H312 . 0.960 no
C31 . H313 . 0.960 no
C32 . C33 . 1.402(9) yes
C32 . O31 . 1.247(9) yes
C33 . C34 . 1.371(9) yes
C33 . H331 . 0.950 no
C34 . C35 . 1.506(9) yes
C34 . O32 . 1.273(9) yes
C35 . C36 . 1.373(9) yes
C35 . C39 . 1.369(9) yes
C36 . C37 . 1.368(9) yes
C36 . H361 . 0.950 no
C37 . N2 . 1.332(9) yes
C37 . H371 . 0.950 no
C38 . C39 . 1.374(9) yes
C38 . N2 . 1.335(9) yes
C38 . H381 . 0.950 no
C39 . H391 . 0.950 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
N1 16_543 Cu1 . N4 . 178.2(8) yes
N1 16_543 Cu1 . O1 . 99.6(8) yes
N4 . Cu1 . O1 . 82.0(8) yes
N1 16_543 Cu1 . O2 . 91.2(11) yes
N4 . Cu1 . O2 . 87.8(10) yes
O1 . Cu1 . O2 . 91.6(9) yes
N1 16_543 Cu1 . O31 . 83.9(7) yes
N4 . Cu1 . O31 . 94.5(8) yes
O1 . Cu1 . O31 . 176.5(10) yes
O2 . Cu1 . O31 . 88.0(8) yes
N1 16_543 Cu1 . O32 . 92.7(10) yes
N4 . Cu1 . O32 . 88.2(9) yes
O1 . Cu1 . O32 . 93.5(8) yes
O2 . Cu1 . O32 . 173.0(12) yes
O31 . Cu1 . O32 . 86.5(9) yes
O11 16_545 Cu2 . N3 15_555 94.7(7) yes
O11 16_545 Cu2 . O12 16_545 87.4(8) yes
N3 15_555 Cu2 . O12 16_545 87.4(9) yes
O11 16_545 Cu2 . N2 . 85.6(7) yes
N3 15_555 Cu2 . N2 . 179.4(9) yes
O12 16_545 Cu2 . N2 . 92.0(10) yes
O11 16_545 Cu2 . O21 . 177.4(8) yes
N3 15_555 Cu2 . O21 . 82.9(7) yes
O12 16_545 Cu2 . O21 . 91.3(8) yes
N2 . Cu2 . O21 . 96.8(7) yes
O11 16_545 Cu2 . O22 . 94.3(8) yes
N3 15_555 Cu2 . O22 . 90.9(10) yes
O12 16_545 Cu2 . O22 . 177.7(8) yes
N2 . Cu2 . O22 . 89.6(9) yes
O21 . Cu2 . O22 . 86.9(8) yes
C2 . C1 . H11 . 110.8 no
C2 . C1 . H12 . 109.5 no
H11 . C1 . H12 . 109.5 no
C2 . C1 . H13 . 108.1 no
H11 . C1 . H13 . 109.5 no
H12 . C1 . H13 . 109.5 no
C1 . C2 . C3 . 118.2(8) yes
C1 . C2 . O1 . 116.2(8) yes
C3 . C2 . O1 . 125.2(8) yes
C2 . C3 . C4 . 125.3(8) yes
C2 . C3 . H31 . 116.4 no
C4 . C3 . H31 . 118.1 no
C3 . C4 . C5 . 119.2(7) yes
C3 . C4 . O2 . 126.4(7) yes
C5 . C4 . O2 . 114.4(7) yes
C4 . C5 . C6 . 121.4(7) yes
C4 . C5 . C9 . 119.3(7) yes
C6 . C5 . C9 . 119.0(6) yes
C5 . C6 . C7 . 119.0(7) yes
C5 . C6 . H61 . 120.8 no
C7 . C6 . H61 . 120.2 no
C6 . C7 . N1 . 120.8(7) yes
C6 . C7 . H71 . 119.9 no
N1 . C7 . H71 . 119.3 no
C9 . C8 . N1 . 120.5(7) yes
C9 . C8 . H81 . 119.6 no
N1 . C8 . H81 . 120.0 no
C8 . C9 . C5 . 119.7(7) yes
C8 . C9 . H91 . 120.4 no
C5 . C9 . H91 . 119.9 no
C12 . C11 . H111 . 110.6 no
C12 . C11 . H112 . 105.8 no
H111 . C11 . H112 . 109.5 no
C12 . C11 . H113 . 111.9 no
H111 . C11 . H113 . 109.5 no
H112 . C11 . H113 . 109.5 no
C11 . C12 . C13 . 118.5(7) yes
C11 . C12 . O11 . 116.0(7) yes
C13 . C12 . O11 . 125.5(7) yes
C12 . C13 . C14 . 125.7(7) yes
C12 . C13 . H131 . 116.3 no
C14 . C13 . H131 . 118.0 no
C13 . C14 . C15 . 119.3(7) yes
C13 . C14 . O12 . 126.3(7) yes
C15 . C14 . O12 . 114.2(7) yes
C14 . C15 . C16 . 121.7(8) yes
C14 . C15 . C19 . 117.8(13) yes
C16 . C15 . C19 . 120.0(12) yes
C15 . C16 . C17 . 119.0(8) yes
C15 . C16 . H161 . 119.6 no
C17 . C16 . H161 . 121.4 no
C16 . C17 . N4 . 120.0(7) yes
C16 . C17 . H171 . 119.0 no
N4 . C17 . H171 . 121.0 no
C19 . C18 . N4 . 120.5(9) yes
C19 . C18 . H181 . 120.6 no
N4 . C18 . H181 . 118.9 no
C18 . C19 . C15 . 119.9(15) yes
C18 . C19 . H191 . 118.8 no
C15 . C19 . H191 . 121.1 no
C22 . C21 . H211 . 108.9 no
C22 . C21 . H212 . 117.9 no
H211 . C21 . H212 . 109.5 no
C22 . C21 . H213 . 101.1 no
H211 . C21 . H213 . 109.5 no
H212 . C21 . H213 . 109.5 no
C21 . C22 . C23 . 117.7(8) yes
C21 . C22 . O21 . 115.8(8) yes
C23 . C22 . O21 . 124.8(8) yes
C22 . C23 . C24 . 126.0(8) yes
C22 . C23 . H231 . 115.8 no
C24 . C23 . H231 . 117.3 no
C23 . C24 . C25 . 118.5(7) yes
C23 . C24 . O22 . 126.1(7) yes
C25 . C24 . O22 . 114.4(7) yes
C24 . C25 . C26 . 120.5(6) yes
C24 . C25 . C29 . 119.6(7) yes
C26 . C25 . C29 . 119.5(6) yes
C25 . C26 . C27 . 118.8(6) yes
C25 . C26 . H261 . 121.3 no
C27 . C26 . H261 . 119.9 no
C26 . C27 . N3 . 121.8(7) yes
C26 . C27 . H271 . 119.8 no
N3 . C27 . H271 . 118.3 no
C29 . C28 . N3 . 121.8(7) yes
C29 . C28 . H281 . 118.3 no
N3 . C28 . H281 . 119.9 no
C28 . C29 . C25 . 119.0(7) yes
C28 . C29 . H291 . 121.2 no
C25 . C29 . H291 . 119.9 no
C32 . C31 . H311 . 109.3 no
C32 . C31 . H312 . 108.8 no
H311 . C31 . H312 . 109.5 no
C32 . C31 . H313 . 110.3 no
H311 . C31 . H313 . 109.5 no
H312 . C31 . H313 . 109.5 no
C31 . C32 . C33 . 117.5(8) yes
C31 . C32 . O31 . 115.7(8) yes
C33 . C32 . O31 . 124.8(8) yes
C32 . C33 . C34 . 126.2(8) yes
C32 . C33 . H331 . 117.4 no
C34 . C33 . H331 . 116.1 no
C33 . C34 . C35 . 119.1(7) yes
C33 . C34 . O32 . 126.2(7) yes
C35 . C34 . O32 . 114.2(7) yes
C34 . C35 . C36 . 119.3(7) yes
C34 . C35 . C39 . 121.0(7) yes
C36 . C35 . C39 . 118.7(6) yes
C35 . C36 . C37 . 119.7(7) yes
C35 . C36 . H361 . 121.1 no
C37 . C36 . H361 . 119.2 no
C36 . C37 . N2 . 121.7(7) yes
C36 . C37 . H371 . 120.1 no
N2 . C37 . H371 . 118.2 no
C39 . C38 . N2 . 121.9(7) yes
C39 . C38 . H381 . 118.3 no
N2 . C38 . H381 . 119.8 no
C38 . C39 . C35 . 119.1(7) yes
C38 . C39 . H391 . 121.3 no
C35 . C39 . H391 . 119.6 no
C7 . N1 . C8 . 121.0(7) yes
C7 . N1 . Cu1 10_553 117.6(12) yes
C8 . N1 . Cu1 10_553 121.4(12) yes
C38 . N2 . C37 . 118.9(7) yes
C38 . N2 . Cu2 . 117.3(11) yes
C37 . N2 . Cu2 . 123.7(11) yes
C27 . N3 . C28 . 119.1(7) yes
C27 . N3 . Cu2 11_554 118.8(11) yes
C28 . N3 . Cu2 11_554 121.5(11) yes
C18 . N4 . C17 . 120.6(8) yes
C18 . N4 . Cu1 . 123.8(12) yes
C17 . N4 . Cu1 . 115.5(12) yes
Cu1 . O1 . C2 . 120.1(13) yes
C4 . O2 . Cu1 . 123.6(13) yes
Cu2 10_555 O11 . C12 . 114.7(15) yes
C14 . O12 . Cu2 10_555 129.5(10) yes
Cu2 . O21 . C22 . 119.7(11) yes
C24 . O22 . Cu2 . 130.3(10) yes
Cu1 . O31 . C32 . 119.3(14) yes
C34 . O32 . Cu1 . 127.7(10) yes



# 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
-31 35 0 x .
-8 8 2 x .
-43 34 1 x .
0 9 3 x .
4 6 1 x .
-10 12 2 x .
6 23 1 x .
-40 29 3 x .
-6 10 2 x .
-7 38 3 x .
0 0 3 x .
2 8 3 x .
-27 44 1 x .
3 9 3 x .
0 0 6 x .
-6 14 1 x .
-10 16 1 x .
11 14 6 x .
2 6 2 x .
8 10 4 x .
-34 21 5 x .
4 12 1 x .
-9 9 3 x .
-11 10 6 x .
-3 9 3 x .
-19 33 5 x .
-14 13 6 x .
-25 17 6 x .
-2 4 3 x .
-7 4 4 x .
-4 22 1 x .
-24 42 3 x .
-7 7 1 x .
-47 33 1 x .
10 18 4 x .
5 5 3 x .
-17 18 1 x .
-19 16 1 x .
0 10 2 x .
-12 12 3 x .
-3 14 1 x .
-14 12 1 x .
-4 6 2 x .
4 8 2 x .
-4 24 2 x .
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_FC70_007_Lab
_database_code_depnum_ccdc_archive 'CCDC 1564961'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2020-06-09 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_audit_creation_date             2016-06-09
_audit_creation_method           CRYSTALS_ver_14.61_build_5965

_oxford_structure_analysis_title 'ST5127_0m in R-3'
_chemical_name_systematic        ?
_chemical_melting_point          ?

#end of refcif 
_cell_length_a                   26.4400(6)
_cell_length_b                   26.4400(6)
_cell_length_c                   7.8045(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4725.0(2)

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3

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            9

# Given Formula = C24 H21.33 Cu1.33 N2.67 O5.33 
# Dc =      1.64 Fooo =   2388.00 Mu =     14.14 M =    517.18
# Found Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.23 FOOO =   1791.00 Mu =     10.60 M =    387.88

_chemical_formula_sum            'C18 H16 Cu1 N2 O4'
_chemical_formula_moiety         'C18 H16 Cu1 N2 O4'
_chemical_compound_source        ?
_chemical_formula_weight         387.88


_cell_measurement_reflns_used    2485
_cell_measurement_theta_min      4
_cell_measurement_theta_max      24
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1791
_exptl_absorpt_coefficient_mu    1.060

# Sheldrick geometric approximatio 0.81 0.90 
_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  0.90
_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_ambient_pressure         70000
_diffrn_reflns_number            5817
_reflns_number_total             1405
_diffrn_reflns_av_R_equivalents  0.043
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 1405 
# Theoretical number of reflections is about 3457 


_diffrn_reflns_theta_min         3.515
_diffrn_reflns_theta_max         24.407
_diffrn_measured_fraction_theta_max 0.814

_diffrn_reflns_theta_full        18.305
_diffrn_measured_fraction_theta_full 0.866


_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_reflns_limit_h_min              -28
_reflns_limit_h_max              11
_reflns_limit_k_min              0
_reflns_limit_k_max              29
_reflns_limit_l_min              0
_reflns_limit_l_max              8

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.69
_refine_diff_density_max         0.81


# 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>-3.0\s(I)
_refine_ls_number_reflns         1402
_refine_ls_number_restraints     126
_refine_ls_number_parameters     115
_oxford_refine_ls_R_factor_ref   0.1011
_refine_ls_wR_factor_ref         0.1693
_refine_ls_goodness_of_fit_ref   1.0000
_refine_ls_shift/su_max          0.0001618
_refine_ls_shift/su_mean         0.0000195


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1402
_refine_ls_R_factor_all          0.1011
_refine_ls_wR_factor_all         0.1693

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                1053
_refine_ls_R_factor_gt           0.0701
_refine_ls_wR_factor_gt          0.1481

# 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, 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: 
 0.372 0.263 -0.541E-01 
;

# 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 0.8333 0.6667 0.6667 0.0460 1.0000 Uani S . . . . .
O2 O 0.7622(2) 0.6349(2) 0.5275(6) 0.0532 1.0000 Uani D U . . . .
C4 C 0.7135(2) 0.5905(3) 0.5679(7) 0.0503 1.0000 Uani D U . . . .
C5 C 0.6656(2) 0.5745(3) 0.4405(7) 0.0562 1.0000 Uani D U . . . .
C6 C 0.6782(3) 0.5942(4) 0.2741(8) 0.0727 1.0000 Uani D U . . . .
C7 C 0.6343(3) 0.5744(4) 0.1541(8) 0.0733 1.0000 Uani D U . . . .
N1 N 0.5784(3) 0.5390(3) 0.1907(7) 0.0622 1.0000 Uani D U . . . .
C9 C 0.5663(3) 0.5223(4) 0.3532(8) 0.0634 1.0000 Uani D U . . . .
C8 C 0.6075(3) 0.5377(3) 0.4797(8) 0.0576 1.0000 Uani D U . . . .
C3 C 0.7028(3) 0.5565(4) 0.7117(9) 0.0691 1.0000 Uani D U . . . .
C2 C 0.7454(3) 0.5584(3) 0.8247(9) 0.0636 1.0000 Uani D U . . . .
O1 O 0.7984(2) 0.5956(2) 0.8205(7) 0.0616 1.0000 Uani D U . . . .
C1 C 0.7261(4) 0.5126(4) 0.9632(12) 0.0961 1.0000 Uani D U . . . .
H61 H 0.7172 0.6208 0.2403 0.0966 1.0000 Uiso R . . . . .
H71 H 0.6440 0.5880 0.0394 0.0900 1.0000 Uiso R . . . . .
H91 H 0.5269 0.4963 0.3844 0.0809 1.0000 Uiso R . . . . .
H81 H 0.5966 0.5244 0.5941 0.0680 1.0000 Uiso R . . . . .
H31 H 0.6630 0.5309 0.7406 0.0882 1.0000 Uiso R . . . . .
H11 H 0.7600 0.5177 1.0287 0.1075 1.0000 Uiso R . . . . .
H12 H 0.6996 0.5179 1.0394 0.1075 1.0000 Uiso R . . . . .
H13 H 0.7056 0.4733 0.9138 0.1075 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.0134673(15)
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 . N1 9_655 2.332(5) yes
Cu1 . N1 10_555 2.332(5) yes
Cu1 . O1 6_666 2.022(5) yes
Cu1 . O2 6_666 1.960(5) yes
Cu1 . O2 . 1.960(5) yes
Cu1 . O1 . 2.022(5) yes
O2 . C4 . 1.276(6) yes
C4 . C5 . 1.494(6) yes
C4 . C3 . 1.376(7) yes
C5 . C6 . 1.377(7) yes
C5 . C8 . 1.380(7) yes
C6 . C7 . 1.375(7) yes
C6 . H61 . 0.950 no
C7 . N1 . 1.327(7) yes
C7 . H71 . 0.950 no
N1 . C9 . 1.328(6) yes
C9 . C8 . 1.373(7) yes
C9 . H91 . 0.950 no
C8 . H81 . 0.950 no
C3 . C2 . 1.413(7) yes
C3 . H31 . 0.950 no
C2 . O1 . 1.246(6) yes
C2 . C1 . 1.508(7) yes
C1 . H11 . 0.980 no
C1 . H12 . 0.980 no
C1 . H13 . 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
N1 9_655 Cu1 . N1 10_555 179.995 yes
N1 9_655 Cu1 . O1 6_666 93.6(2) yes
N1 10_555 Cu1 . O1 6_666 86.4(2) yes
N1 9_655 Cu1 . O2 6_666 89.9(2) yes
N1 10_555 Cu1 . O2 6_666 90.1(2) yes
O1 6_666 Cu1 . O2 6_666 92.1(2) yes
N1 9_655 Cu1 . O2 . 90.1(2) yes
N1 10_555 Cu1 . O2 . 89.9(2) yes
O1 6_666 Cu1 . O2 . 87.9(2) yes
O2 6_666 Cu1 . O2 . 179.994 yes
N1 9_655 Cu1 . O1 . 86.4(2) yes
N1 10_555 Cu1 . O1 . 93.6(2) yes
O1 6_666 Cu1 . O1 . 179.994 yes
O2 6_666 Cu1 . O1 . 87.9(2) yes
O2 . Cu1 . O1 . 92.1(2) yes
Cu1 . O2 . C4 . 124.7(4) yes
O2 . C4 . C5 . 114.7(4) yes
O2 . C4 . C3 . 125.9(5) yes
C5 . C4 . C3 . 119.3(4) yes
C4 . C5 . C6 . 120.7(4) yes
C4 . C5 . C8 . 122.6(4) yes
C6 . C5 . C8 . 116.7(4) yes
C5 . C6 . C7 . 120.0(5) yes
C5 . C6 . H61 . 120.6 no
C7 . C6 . H61 . 119.3 no
C6 . C7 . N1 . 123.5(5) yes
C6 . C7 . H71 . 118.7 no
N1 . C7 . H71 . 117.7 no
Cu1 16_545 N1 . C7 . 127.2(4) yes
Cu1 16_545 N1 . C9 . 116.8(4) yes
C7 . N1 . C9 . 116.0(5) yes
N1 . C9 . C8 . 124.4(5) yes
N1 . C9 . H91 . 118.6 no
C8 . C9 . H91 . 116.9 no
C5 . C8 . C9 . 119.2(5) yes
C5 . C8 . H81 . 119.6 no
C9 . C8 . H81 . 121.2 no
C4 . C3 . C2 . 125.9(5) yes
C4 . C3 . H31 . 116.9 no
C2 . C3 . H31 . 117.2 no
C3 . C2 . O1 . 125.0(5) yes
C3 . C2 . C1 . 118.3(5) yes
O1 . C2 . C1 . 116.7(5) yes
C2 . O1 . Cu1 . 124.1(4) yes
C2 . C1 . H11 . 110.1 no
C2 . C1 . H12 . 107.6 no
H11 . C1 . H12 . 109.5 no
C2 . C1 . H13 . 110.7 no
H11 . C1 . H13 . 109.5 no
H12 . C1 . H13 . 109.5 no



# 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
-8 16 0 x .
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_FC70_014_Lab
_database_code_depnum_ccdc_archive 'CCDC 1564962'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2020-06-09 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_audit_creation_date             2016-06-09
_audit_creation_method           CRYSTALS_ver_14.61_build_5965

_oxford_structure_analysis_title 'ST5129_0m in R-3'
_chemical_name_systematic        ?
_chemical_melting_point          ?

#end of refcif 
_cell_length_a                   26.3304(7)
_cell_length_b                   26.3304(7)
_cell_length_c                   7.7955(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4680.5(3)

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3

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            9

# Given Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.24 Fooo =   1791.00 Mu =     10.70 M =    387.88
# Found Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.24 FOOO =   1791.00 Mu =     10.70 M =    387.88

_chemical_formula_sum            'C18 H16 Cu1 N2 O4'
_chemical_formula_moiety         'C18 H16 Cu1 N2 O4'
_chemical_compound_source        ?
_chemical_formula_weight         387.88


_cell_measurement_reflns_used    2411
_cell_measurement_theta_min      3
_cell_measurement_theta_max      24
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1791
_exptl_absorpt_coefficient_mu    1.070

# Sheldrick geometric approximatio 0.81 0.90 
_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  0.90
_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_ambient_pressure         140000
_diffrn_reflns_number            5756
_reflns_number_total             1393
_diffrn_reflns_av_R_equivalents  0.044
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 1393 
# Theoretical number of reflections is about 3419 


_diffrn_reflns_theta_min         3.166
_diffrn_reflns_theta_max         24.393
_diffrn_measured_fraction_theta_max 0.814

_diffrn_reflns_theta_full        18.294
_diffrn_measured_fraction_theta_full 0.865


_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_reflns_limit_h_min              -28
_reflns_limit_h_max              11
_reflns_limit_k_min              0
_reflns_limit_k_max              29
_reflns_limit_l_min              0
_reflns_limit_l_max              8

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.65
_refine_diff_density_max         0.61


# 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>-3.0\s(I)
_refine_ls_number_reflns         1389
_refine_ls_number_restraints     126
_refine_ls_number_parameters     115
_oxford_refine_ls_R_factor_ref   0.0949
_refine_ls_wR_factor_ref         0.1753
_refine_ls_goodness_of_fit_ref   1.0493
_refine_ls_shift/su_max          0.0001149
_refine_ls_shift/su_mean         0.0000140


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1389
_refine_ls_R_factor_all          0.0949
_refine_ls_wR_factor_all         0.1753

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                1034
_refine_ls_R_factor_gt           0.0701
_refine_ls_wR_factor_gt          0.1510

# 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, 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: 
 3.75 4.14 0.717 
;

# 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 0.8333 0.6667 0.6667 0.0460 1.0000 Uani S . . . . .
O2 O 0.7614(2) 0.6344(2) 0.5270(6) 0.0535 1.0000 Uani D U . . . .
C4 C 0.7127(3) 0.5899(3) 0.5670(8) 0.0557 1.0000 Uani D U . . . .
C5 C 0.6644(3) 0.5738(3) 0.4401(8) 0.0559 1.0000 Uani D U . . . .
C6 C 0.6773(3) 0.5934(4) 0.2728(9) 0.0692 1.0000 Uani D U . . . .
C7 C 0.6337(3) 0.5740(4) 0.1520(9) 0.0747 1.0000 Uani D U . . . .
N1 N 0.5774(3) 0.5380(3) 0.1886(7) 0.0608 1.0000 Uani D U . . . .
C9 C 0.5649(3) 0.5204(4) 0.3513(8) 0.0690 1.0000 Uani D U . . . .
C8 C 0.6058(3) 0.5372(4) 0.4799(8) 0.0596 1.0000 Uani D U . . . .
C3 C 0.7019(3) 0.5555(4) 0.7107(10) 0.0801 1.0000 Uani D U . . . .
C2 C 0.7442(3) 0.5576(3) 0.8246(9) 0.0657 1.0000 Uani D U . . . .
O1 O 0.7978(2) 0.5942(3) 0.8203(7) 0.0620 1.0000 Uani D U . . . .
C1 C 0.7243(5) 0.5108(5) 0.9610(13) 0.1020 1.0000 Uani D U . . . .
H61 H 0.7165 0.6208 0.2409 0.0705 1.0000 Uiso R . . . . .
H71 H 0.6441 0.5864 0.0366 0.0708 1.0000 Uiso R . . . . .
H91 H 0.5249 0.4960 0.3823 0.0710 1.0000 Uiso R . . . . .
H81 H 0.5945 0.5241 0.5944 0.0691 1.0000 Uiso R . . . . .
H31 H 0.6620 0.5281 0.7352 0.0726 1.0000 Uiso R . . . . .
H11 H 0.7580 0.5175 1.0311 0.0781 1.0000 Uiso R . . . . .
H12 H 0.6947 0.5122 1.0339 0.0781 1.0000 Uiso R . . . . .
H13 H 0.7072 0.4721 0.9063 0.0781 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.05864(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 . N1 9_655 2.297(6) yes
Cu1 . N1 10_555 2.297(6) yes
Cu1 . O1 6_666 2.040(6) yes
Cu1 . O2 6_666 1.972(5) yes
Cu1 . O2 . 1.972(5) yes
Cu1 . O1 . 2.040(6) yes
O2 . C4 . 1.268(6) yes
C4 . C5 . 1.497(6) yes
C4 . C3 . 1.378(7) yes
C5 . C6 . 1.382(7) yes
C5 . C8 . 1.384(7) yes
C6 . C7 . 1.371(7) yes
C6 . H61 . 0.950 no
C7 . N1 . 1.331(7) yes
C7 . H71 . 0.950 no
N1 . C9 . 1.334(7) yes
C9 . C8 . 1.373(7) yes
C9 . H91 . 0.950 no
C8 . H81 . 0.950 no
C3 . C2 . 1.404(7) yes
C3 . H31 . 0.950 no
C2 . O1 . 1.250(7) yes
C2 . C1 . 1.509(7) yes
C1 . H11 . 0.980 no
C1 . H12 . 0.980 no
C1 . H13 . 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
N1 9_655 Cu1 . N1 10_555 179.995 yes
N1 9_655 Cu1 . O1 6_666 93.1(2) yes
N1 10_555 Cu1 . O1 6_666 86.9(2) yes
N1 9_655 Cu1 . O2 6_666 89.6(2) yes
N1 10_555 Cu1 . O2 6_666 90.4(2) yes
O1 6_666 Cu1 . O2 6_666 91.6(2) yes
N1 9_655 Cu1 . O2 . 90.4(2) yes
N1 10_555 Cu1 . O2 . 89.6(2) yes
O1 6_666 Cu1 . O2 . 88.4(2) yes
O2 6_666 Cu1 . O2 . 179.994 yes
N1 9_655 Cu1 . O1 . 86.9(2) yes
N1 10_555 Cu1 . O1 . 93.1(2) yes
O1 6_666 Cu1 . O1 . 179.994 yes
O2 6_666 Cu1 . O1 . 88.4(2) yes
O2 . Cu1 . O1 . 91.6(2) yes
Cu1 . O2 . C4 . 124.9(4) yes
O2 . C4 . C5 . 115.0(4) yes
O2 . C4 . C3 . 126.1(5) yes
C5 . C4 . C3 . 118.9(5) yes
C4 . C5 . C6 . 120.1(4) yes
C4 . C5 . C8 . 122.9(4) yes
C6 . C5 . C8 . 116.9(5) yes
C5 . C6 . C7 . 120.3(5) yes
C5 . C6 . H61 . 120.2 no
C7 . C6 . H61 . 119.5 no
C6 . C7 . N1 . 123.1(5) yes
C6 . C7 . H71 . 118.6 no
N1 . C7 . H71 . 118.3 no
Cu1 16_545 N1 . C7 . 127.1(4) yes
Cu1 16_545 N1 . C9 . 116.5(4) yes
C7 . N1 . C9 . 116.4(5) yes
N1 . C9 . C8 . 124.4(5) yes
N1 . C9 . H91 . 118.3 no
C8 . C9 . H91 . 117.2 no
C5 . C8 . C9 . 118.8(5) yes
C5 . C8 . H81 . 120.1 no
C9 . C8 . H81 . 121.1 no
C4 . C3 . C2 . 126.1(5) yes
C4 . C3 . H31 . 116.7 no
C2 . C3 . H31 . 117.2 no
C3 . C2 . O1 . 125.5(5) yes
C3 . C2 . C1 . 117.9(5) yes
O1 . C2 . C1 . 116.6(5) yes
C2 . O1 . Cu1 . 123.5(4) yes
C2 . C1 . H11 . 109.4 no
C2 . C1 . H12 . 109.6 no
H11 . C1 . H12 . 109.5 no
C2 . C1 . H13 . 109.5 no
H11 . C1 . H13 . 109.5 no
H12 . C1 . H13 . 109.5 no


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_FC70_127_Lab
_database_code_depnum_ccdc_archive 'CCDC 1564965'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2020-06-09 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_audit_creation_date             2016-06-10
_audit_creation_method           CRYSTALS_ver_14.61_build_5965

_oxford_structure_analysis_title 'st5136_0m in R-3'
_chemical_name_systematic        ?
_chemical_melting_point          ?

#end of refcif 
_cell_length_a                   25.342(2)
_cell_length_b                   25.342(2)
_cell_length_c                   7.7011(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4283.1(8)

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_space_group_name_Hall  '-R 3  '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3

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            9

# Given Formula = C20 H20 Cu1 N10 O10 
# Dc =      2.18 Fooo =   2871.00 Mu =     12.49 M =    623.99
# Found Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.35 FOOO =   1791.00 Mu =     11.70 M =    387.88

_chemical_formula_sum            'C18 H16 Cu1 N2 O4'
_chemical_formula_moiety         'C18 H16 Cu1 N2 O4'
_chemical_compound_source        ?
_chemical_formula_weight         387.88


_cell_measurement_reflns_used    1468
_cell_measurement_theta_min      3
_cell_measurement_theta_max      19
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1791
_exptl_absorpt_coefficient_mu    1.170

# Sheldrick geometric approximatio 0.79 0.89 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_T_max  0.89
_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_ambient_pressure         1270000
_diffrn_reflns_number            3986
_reflns_number_total             915
_diffrn_reflns_av_R_equivalents  0.092
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 915 
# Theoretical number of reflections is about 1992 


_diffrn_reflns_theta_min         3.216
_diffrn_reflns_theta_max         20.809
_diffrn_measured_fraction_theta_max 0.911

_diffrn_reflns_theta_full        15.607
_diffrn_measured_fraction_theta_full 0.935


_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_reflns_limit_h_min              -24
_reflns_limit_h_max              10
_reflns_limit_k_min              0
_reflns_limit_k_max              24
_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,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.97
_refine_diff_density_max         0.88


# 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>-3.0\s(I)
_refine_ls_number_reflns         911
_refine_ls_number_restraints     126
_refine_ls_number_parameters     115
_oxford_refine_ls_R_factor_ref   0.1318
_refine_ls_wR_factor_ref         0.2454
_refine_ls_goodness_of_fit_ref   1.0094
_refine_ls_shift/su_max          0.0000963
_refine_ls_shift/su_mean         0.0000115


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        911
_refine_ls_R_factor_all          0.1318
_refine_ls_wR_factor_all         0.2454

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                596
_refine_ls_R_factor_gt           0.0871
_refine_ls_wR_factor_gt          0.1924

# 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, 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: 
 8.58 10.7 2.95 
;

# 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 0.8333 0.6667 0.6667 0.0634 1.0000 Uani S . . . . .
O2 O 0.7571(3) 0.6337(4) 0.5308(11) 0.0712 1.0000 Uani D U . . . .
C4 C 0.7063(3) 0.5874(4) 0.5724(11) 0.0666 1.0000 Uani D U . . . .
C5 C 0.6567(3) 0.5713(5) 0.4420(11) 0.0677 1.0000 Uani D U . . . .
C6 C 0.6710(4) 0.5928(6) 0.2743(13) 0.0790 1.0000 Uani D U . . . .
C7 C 0.6270(4) 0.5729(6) 0.1483(12) 0.0841 1.0000 Uani D U . . . .
N1 N 0.5685(4) 0.5337(4) 0.1810(11) 0.0634 1.0000 Uani D U . . . .
C9 C 0.5549(4) 0.5121(5) 0.3427(13) 0.0709 1.0000 Uani D U . . . .
C8 C 0.5962(4) 0.5289(5) 0.4749(12) 0.0749 1.0000 Uani D U . . . .
C3 C 0.6933(4) 0.5531(6) 0.7209(15) 0.0896 1.0000 Uani D U . . . .
C2 C 0.7351(4) 0.5501(6) 0.8354(16) 0.0875 1.0000 Uani D U . . . .
O1 O 0.7918(4) 0.5842(4) 0.8288(12) 0.0824 1.0000 Uani D U . . . .
C1 C 0.7106(6) 0.5016(8) 0.975(2) 0.1202 1.0000 Uani D U . . . .
H61 H 0.7118 0.6220 0.2459 0.0986 1.0000 Uiso R . . . . .
H71 H 0.6384 0.5888 0.0341 0.0967 1.0000 Uiso R . . . . .
H91 H 0.5133 0.4850 0.3698 0.0801 1.0000 Uiso R . . . . .
H81 H 0.5840 0.5105 0.5862 0.0884 1.0000 Uiso R . . . . .
H31 H 0.6515 0.5279 0.7486 0.0996 1.0000 Uiso R . . . . .
H11 H 0.7446 0.5059 1.0458 0.1390 1.0000 Uiso R . . . . .
H12 H 0.6810 0.5050 1.0488 0.1390 1.0000 Uiso R . . . . .
H13 H 0.6909 0.4618 0.9173 0.1390 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.07053(7)
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 6_666 2.200(9) yes
Cu1 . N1 9_655 2.051(8) yes
Cu1 . N1 10_555 2.051(8) yes
Cu1 . O2 6_666 1.977(7) yes
Cu1 . O2 . 1.977(7) yes
Cu1 . O1 . 2.200(9) yes
O2 . C4 . 1.276(7) yes
C4 . C5 . 1.497(7) yes
C4 . C3 . 1.374(8) yes
C5 . C6 . 1.377(8) yes
C5 . C8 . 1.386(8) yes
C6 . C7 . 1.370(8) yes
C6 . H61 . 0.949 no
C7 . N1 . 1.333(8) yes
C7 . H71 . 0.950 no
N1 . C9 . 1.334(8) yes
C9 . C8 . 1.367(8) yes
C9 . H91 . 0.949 no
C8 . H81 . 0.950 no
C3 . C2 . 1.409(8) yes
C3 . H31 . 0.949 no
C2 . O1 . 1.254(8) yes
C2 . C1 . 1.510(8) yes
C1 . H11 . 0.980 no
C1 . H12 . 0.980 no
C1 . H13 . 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
O1 6_666 Cu1 . N1 9_655 94.7(4) yes
O1 6_666 Cu1 . N1 10_555 85.3(4) yes
N1 9_655 Cu1 . N1 10_555 179.994 yes
O1 6_666 Cu1 . O2 6_666 89.8(3) yes
N1 9_655 Cu1 . O2 6_666 89.3(4) yes
N1 10_555 Cu1 . O2 6_666 90.7(4) yes
O1 6_666 Cu1 . O2 . 90.2(3) yes
N1 9_655 Cu1 . O2 . 90.7(4) yes
N1 10_555 Cu1 . O2 . 89.3(4) yes
O2 6_666 Cu1 . O2 . 179.994 yes
O1 6_666 Cu1 . O1 . 179.995 yes
N1 9_655 Cu1 . O1 . 85.3(4) yes
N1 10_555 Cu1 . O1 . 94.7(4) yes
O2 6_666 Cu1 . O1 . 90.2(3) yes
O2 . Cu1 . O1 . 89.8(3) yes
Cu1 . O2 . C4 . 125.4(5) yes
O2 . C4 . C5 . 114.0(5) yes
O2 . C4 . C3 . 127.1(6) yes
C5 . C4 . C3 . 118.9(5) yes
C4 . C5 . C6 . 120.1(5) yes
C4 . C5 . C8 . 122.7(5) yes
C6 . C5 . C8 . 116.7(5) yes
C5 . C6 . C7 . 120.9(6) yes
C5 . C6 . H61 . 119.6 no
C7 . C6 . H61 . 119.5 no
C6 . C7 . N1 . 122.5(6) yes
C6 . C7 . H71 . 118.8 no
N1 . C7 . H71 . 118.7 no
C7 . N1 . Cu1 16_545 125.2(6) yes
C7 . N1 . C9 . 116.5(6) yes
Cu1 16_545 N1 . C9 . 118.2(6) yes
N1 . C9 . C8 . 124.5(6) yes
N1 . C9 . H91 . 117.9 no
C8 . C9 . H91 . 117.5 no
C5 . C8 . C9 . 118.9(6) yes
C5 . C8 . H81 . 120.5 no
C9 . C8 . H81 . 120.6 no
C4 . C3 . C2 . 127.4(6) yes
C4 . C3 . H31 . 116.5 no
C2 . C3 . H31 . 116.1 no
C3 . C2 . O1 . 124.8(6) yes
C3 . C2 . C1 . 118.3(6) yes
O1 . C2 . C1 . 116.9(6) yes
Cu1 . O1 . C2 . 121.1(6) yes
C2 . C1 . H11 . 109.1 no
C2 . C1 . H12 . 111.3 no
H11 . C1 . H12 . 109.4 no
C2 . C1 . H13 . 108.0 no
H11 . C1 . H13 . 109.5 no
H12 . C1 . H13 . 109.5 no


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_FC70_033_Lab
_database_code_depnum_ccdc_archive 'CCDC 1564963'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2020-06-09 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_audit_creation_date             2016-06-10
_audit_creation_method           CRYSTALS_ver_14.61_build_5965

_oxford_structure_analysis_title 'st5130_0m in R-3'
_chemical_name_systematic        ?
_chemical_melting_point          ?

#end of refcif 
_cell_length_a                   26.0243(5)
_cell_length_b                   26.0243(5)
_cell_length_c                   7.7622(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4552.7(2)

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3

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            9

# Given Formula = C10 H10 Cu2 N10 O10 
# Dc =      1.83 Fooo =   2502.00 Mu =     21.75 M =    557.34
# Found Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.27 FOOO =   1791.00 Mu =     11.00 M =    387.88

_chemical_formula_sum            'C18 H16 Cu1 N2 O4'
_chemical_formula_moiety         'C18 H16 Cu1 N2 O4'
_chemical_compound_source        ?
_chemical_formula_weight         387.88


_cell_measurement_reflns_used    2111
_cell_measurement_theta_min      4
_cell_measurement_theta_max      23
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1791
_exptl_absorpt_coefficient_mu    1.100

# Sheldrick geometric approximatio 0.80 0.90 
_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  0.90
_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_ambient_pressure         330000
_diffrn_reflns_number            6310
_reflns_number_total             1561
_diffrn_reflns_av_R_equivalents  0.054
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 1561 
# Theoretical number of reflections is about 4140 


_diffrn_reflns_theta_min         3.551
_diffrn_reflns_theta_max         26.376
_diffrn_measured_fraction_theta_max 0.755

_diffrn_reflns_theta_full        25.057
_diffrn_measured_fraction_theta_full 0.771


_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       8
_reflns_limit_h_min              -29
_reflns_limit_h_max              11
_reflns_limit_k_min              0
_reflns_limit_k_max              30
_reflns_limit_l_min              0
_reflns_limit_l_max              9

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.24
_refine_diff_density_max         1.23


# 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>-3.0\s(I)
_refine_ls_number_reflns         1557
_refine_ls_number_restraints     126
_refine_ls_number_parameters     115
_oxford_refine_ls_R_factor_ref   0.1366
_refine_ls_wR_factor_ref         0.1873
_refine_ls_goodness_of_fit_ref   1.1468
_refine_ls_shift/su_max          0.0001067
_refine_ls_shift/su_mean         0.0000146


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1557
_refine_ls_R_factor_all          0.1366
_refine_ls_wR_factor_all         0.1873

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                1040
_refine_ls_R_factor_gt           0.0888
_refine_ls_wR_factor_gt          0.1667

# 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, 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: 
 0.758 0.916 0.193 
;

# 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 0.8333 0.6667 0.6667 0.0482 1.0000 Uani S . . . . .
O2 O 0.7601(2) 0.6339(2) 0.5292(6) 0.0552 1.0000 Uani D U . . . .
C4 C 0.7104(3) 0.5892(3) 0.5688(8) 0.0556 1.0000 Uani D U . . . .
C5 C 0.6618(3) 0.5726(3) 0.4393(7) 0.0557 1.0000 Uani D U . . . .
C6 C 0.6750(3) 0.5924(4) 0.2709(9) 0.0733 1.0000 Uani D U . . . .
C7 C 0.6303(3) 0.5731(4) 0.1501(9) 0.0724 1.0000 Uani D U . . . .
N1 N 0.5737(3) 0.5354(3) 0.1855(7) 0.0641 1.0000 Uani D U . . . .
C9 C 0.5607(3) 0.5179(4) 0.3482(8) 0.0656 1.0000 Uani D U . . . .
C8 C 0.6024(3) 0.5351(4) 0.4766(8) 0.0638 1.0000 Uani D U . . . .
C3 C 0.6989(3) 0.5542(4) 0.7135(10) 0.0769 1.0000 Uani D U . . . .
C2 C 0.7413(3) 0.5540(3) 0.8266(9) 0.0673 1.0000 Uani D U . . . .
O1 O 0.7950(2) 0.5897(3) 0.8225(7) 0.0659 1.0000 Uani D U . . . .
C1 C 0.7196(4) 0.5067(4) 0.9634(12) 0.1001 1.0000 Uani D U . . . .
H61 H 0.7148 0.6198 0.2396 0.0808 1.0000 Uiso R . . . . .
H71 H 0.6412 0.5863 0.0348 0.0795 1.0000 Uiso R . . . . .
H91 H 0.5203 0.4916 0.3765 0.0854 1.0000 Uiso R . . . . .
H81 H 0.5906 0.5205 0.5904 0.0767 1.0000 Uiso R . . . . .
H31 H 0.6586 0.5253 0.7340 0.0914 1.0000 Uiso R . . . . .
H11 H 0.7531 0.5129 1.0357 0.1156 1.0000 Uiso R . . . . .
H12 H 0.6896 0.5088 1.0349 0.1156 1.0000 Uiso R . . . . .
H13 H 0.7020 0.4675 0.9087 0.1156 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.0108943(13)
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 . N1 9_655 2.198(6) yes
Cu1 . N1 10_555 2.198(6) yes
Cu1 . O1 6_666 2.114(6) yes
Cu1 . O2 6_666 1.969(5) yes
Cu1 . O2 . 1.969(5) yes
Cu1 . O1 . 2.114(6) yes
O2 . C4 . 1.270(6) yes
C4 . C5 . 1.500(6) yes
C4 . C3 . 1.383(7) yes
C5 . C6 . 1.383(7) yes
C5 . C8 . 1.384(7) yes
C6 . C7 . 1.378(7) yes
C6 . H61 . 0.950 no
C7 . N1 . 1.328(7) yes
C7 . H71 . 0.950 no
N1 . C9 . 1.328(6) yes
C9 . C8 . 1.374(7) yes
C9 . H91 . 0.950 no
C8 . H81 . 0.950 no
C3 . C2 . 1.412(7) yes
C3 . H31 . 0.950 no
C2 . O1 . 1.232(6) yes
C2 . C1 . 1.506(7) yes
C1 . H11 . 0.980 no
C1 . H12 . 0.980 no
C1 . H13 . 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
N1 9_655 Cu1 . N1 10_555 179.995 yes
N1 9_655 Cu1 . O1 6_666 93.0(3) yes
N1 10_555 Cu1 . O1 6_666 87.0(3) yes
N1 9_655 Cu1 . O2 6_666 89.0(2) yes
N1 10_555 Cu1 . O2 6_666 91.0(2) yes
O1 6_666 Cu1 . O2 6_666 90.2(2) yes
N1 9_655 Cu1 . O2 . 91.0(2) yes
N1 10_555 Cu1 . O2 . 89.0(2) yes
O1 6_666 Cu1 . O2 . 89.8(2) yes
O2 6_666 Cu1 . O2 . 179.994 yes
N1 9_655 Cu1 . O1 . 87.0(3) yes
N1 10_555 Cu1 . O1 . 93.0(3) yes
O1 6_666 Cu1 . O1 . 179.995 yes
O2 6_666 Cu1 . O1 . 89.8(2) yes
O2 . Cu1 . O1 . 90.2(2) yes
Cu1 . O2 . C4 . 126.0(4) yes
O2 . C4 . C5 . 115.3(5) yes
O2 . C4 . C3 . 125.8(5) yes
C5 . C4 . C3 . 118.8(4) yes
C4 . C5 . C6 . 120.6(4) yes
C4 . C5 . C8 . 123.1(4) yes
C6 . C5 . C8 . 116.2(4) yes
C5 . C6 . C7 . 120.0(5) yes
C5 . C6 . H61 . 119.7 no
C7 . C6 . H61 . 120.2 no
C6 . C7 . N1 . 123.4(5) yes
C6 . C7 . H71 . 117.7 no
N1 . C7 . H71 . 118.8 no
Cu1 16_545 N1 . C7 . 126.0(4) yes
Cu1 16_545 N1 . C9 . 117.4(4) yes
C7 . N1 . C9 . 116.6(5) yes
N1 . C9 . C8 . 123.6(5) yes
N1 . C9 . H91 . 117.9 no
C8 . C9 . H91 . 118.5 no
C5 . C8 . C9 . 120.0(5) yes
C5 . C8 . H81 . 120.0 no
C9 . C8 . H81 . 120.0 no
C4 . C3 . C2 . 126.6(5) yes
C4 . C3 . H31 . 116.5 no
C2 . C3 . H31 . 116.7 no
C3 . C2 . O1 . 125.0(5) yes
C3 . C2 . C1 . 117.8(5) yes
O1 . C2 . C1 . 117.2(5) yes
Cu1 . O1 . C2 . 123.4(4) yes
C2 . C1 . H11 . 109.2 no
C2 . C1 . H12 . 109.7 no
H11 . C1 . H12 . 109.5 no
C2 . C1 . H13 . 109.5 no
H11 . C1 . H13 . 109.5 no
H12 . C1 . H13 . 109.5 no


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_FC70_088_Lab
_database_code_depnum_ccdc_archive 'CCDC 1564964'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2020-06-09 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_audit_creation_date             2016-06-10
_audit_creation_method           CRYSTALS_ver_14.61_build_5965

_oxford_structure_analysis_title 'st5133_0m in R-3'
_chemical_name_systematic        ?
_chemical_melting_point          ?

#end of refcif 
_cell_length_a                   25.4689(16)
_cell_length_b                   25.4689(16)
_cell_length_c                   7.7069(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4329.4(6)

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3

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            9

# Given Formula = C10 H10 Cu2 N10 O10 
# Dc =      1.92 Fooo =   2502.00 Mu =     22.87 M =    557.34
# Found Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.34 FOOO =   1791.00 Mu =     11.57 M =    387.88

_chemical_formula_sum            'C18 H16 Cu1 N2 O4'
_chemical_formula_moiety         'C18 H16 Cu1 N2 O4'
_chemical_compound_source        ?
_chemical_formula_weight         387.88


_cell_measurement_reflns_used    1430
_cell_measurement_theta_min      3
_cell_measurement_theta_max      19
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1791
_exptl_absorpt_coefficient_mu    1.157

# Sheldrick geometric approximatio 0.79 0.89 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_T_max  0.89
_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_ambient_pressure         880000
_diffrn_reflns_number            3989
_reflns_number_total             927
_diffrn_reflns_av_R_equivalents  0.097
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 927 
# Theoretical number of reflections is about 2017 


_diffrn_reflns_theta_min         3.225
_diffrn_reflns_theta_max         20.824
_diffrn_measured_fraction_theta_max 0.920

_diffrn_reflns_theta_full        15.618
_diffrn_measured_fraction_theta_full 0.941


_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_reflns_limit_h_min              -24
_reflns_limit_h_max              10
_reflns_limit_k_min              0
_reflns_limit_k_max              24
_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,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.48
_refine_diff_density_max         1.13


# 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>-3.0\s(I)
_refine_ls_number_reflns         923
_refine_ls_number_restraints     126
_refine_ls_number_parameters     115
_oxford_refine_ls_R_factor_ref   0.1688
_refine_ls_wR_factor_ref         0.3484
_refine_ls_goodness_of_fit_ref   0.9832
_refine_ls_shift/su_max          0.0000643
_refine_ls_shift/su_mean         0.0000078


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        923
_refine_ls_R_factor_all          0.1688
_refine_ls_wR_factor_all         0.3484

# 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           0.1229
_refine_ls_wR_factor_gt          0.2935

# 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, 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: 
 11.7 15.1 4.14 
;

# 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 0.8333 0.6667 0.6667 0.0612 1.0000 Uani S . . . . .
O2 O 0.7577(4) 0.6349(4) 0.5302(13) 0.0668 1.0000 Uani D U . . . .
C4 C 0.7073(4) 0.5885(5) 0.5692(13) 0.0651 1.0000 Uani D U . . . .
C5 C 0.6578(4) 0.5723(6) 0.4392(12) 0.0676 1.0000 Uani D U . . . .
C6 C 0.6713(4) 0.5945(7) 0.2715(14) 0.0789 1.0000 Uani D U . . . .
C7 C 0.6272(5) 0.5718(7) 0.1456(14) 0.0812 1.0000 Uani D U . . . .
N1 N 0.5692(4) 0.5331(5) 0.1790(13) 0.0649 1.0000 Uani D U . . . .
C9 C 0.5562(4) 0.5130(7) 0.3423(15) 0.0740 1.0000 Uani D U . . . .
C8 C 0.5980(4) 0.5306(7) 0.4733(14) 0.0757 1.0000 Uani D U . . . .
C3 C 0.6947(4) 0.5527(7) 0.7137(18) 0.0863 1.0000 Uani D U . . . .
C2 C 0.7360(4) 0.5524(7) 0.8334(18) 0.0815 1.0000 Uani D U . . . .
O1 O 0.7923(4) 0.5863(5) 0.8279(15) 0.0779 1.0000 Uani D U . . . .
C1 C 0.7115(7) 0.5036(9) 0.970(3) 0.1078 1.0000 Uani D U . . . .
H61 H 0.7117 0.6244 0.2430 0.0874 1.0000 Uiso R . . . . .
H71 H 0.6387 0.5854 0.0296 0.0801 1.0000 Uiso R . . . . .
H91 H 0.5151 0.4851 0.3692 0.0827 1.0000 Uiso R . . . . .
H81 H 0.5854 0.5160 0.5880 0.0783 1.0000 Uiso R . . . . .
H31 H 0.6530 0.5264 0.7384 0.0887 1.0000 Uiso R . . . . .
H11 H 0.7449 0.5071 1.0415 0.1104 1.0000 Uiso R . . . . .
H12 H 0.6819 0.5069 1.0435 0.1104 1.0000 Uiso R . . . . .
H13 H 0.6918 0.4643 0.9107 0.1104 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.06339(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 6_666 2.164(11) yes
Cu1 . N1 9_655 2.057(9) yes
Cu1 . N1 10_555 2.057(9) yes
Cu1 . O2 6_666 1.978(9) yes
Cu1 . O2 . 1.978(9) yes
Cu1 . O1 . 2.164(11) yes
O2 . C4 . 1.271(8) yes
C4 . C5 . 1.497(8) yes
C4 . C3 . 1.373(8) yes
C5 . C6 . 1.384(8) yes
C5 . C8 . 1.380(8) yes
C6 . C7 . 1.374(8) yes
C6 . H61 . 0.950 no
C7 . N1 . 1.329(8) yes
C7 . H71 . 0.950 no
N1 . C9 . 1.336(8) yes
C9 . C8 . 1.369(8) yes
C9 . H91 . 0.950 no
C8 . H81 . 0.950 no
C3 . C2 . 1.402(8) yes
C3 . H31 . 0.950 no
C2 . O1 . 1.251(8) yes
C2 . C1 . 1.504(9) yes
C1 . H11 . 0.980 no
C1 . H12 . 0.980 no
C1 . H13 . 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
O1 6_666 Cu1 . N1 9_655 94.3(5) yes
O1 6_666 Cu1 . N1 10_555 85.7(5) yes
N1 9_655 Cu1 . N1 10_555 179.994 yes
O1 6_666 Cu1 . O2 6_666 90.4(4) yes
N1 9_655 Cu1 . O2 6_666 89.6(4) yes
N1 10_555 Cu1 . O2 6_666 90.4(4) yes
O1 6_666 Cu1 . O2 . 89.6(4) yes
N1 9_655 Cu1 . O2 . 90.4(4) yes
N1 10_555 Cu1 . O2 . 89.6(4) yes
O2 6_666 Cu1 . O2 . 179.994 yes
O1 6_666 Cu1 . O1 . 179.995 yes
N1 9_655 Cu1 . O1 . 85.7(5) yes
N1 10_555 Cu1 . O1 . 94.3(5) yes
O2 6_666 Cu1 . O1 . 89.6(4) yes
O2 . Cu1 . O1 . 90.4(4) yes
Cu1 . O2 . C4 . 125.4(6) yes
O2 . C4 . C5 . 114.7(6) yes
O2 . C4 . C3 . 126.9(6) yes
C5 . C4 . C3 . 118.4(5) yes
C4 . C5 . C6 . 120.6(6) yes
C4 . C5 . C8 . 122.6(5) yes
C6 . C5 . C8 . 116.5(5) yes
C5 . C6 . C7 . 120.3(6) yes
C5 . C6 . H61 . 119.5 no
C7 . C6 . H61 . 120.2 no
C6 . C7 . N1 . 123.2(6) yes
C6 . C7 . H71 . 118.2 no
N1 . C7 . H71 . 118.6 no
C7 . N1 . Cu1 16_545 125.5(6) yes
C7 . N1 . C9 . 115.9(6) yes
Cu1 16_545 N1 . C9 . 118.5(6) yes
N1 . C9 . C8 . 124.5(6) yes
N1 . C9 . H91 . 117.5 no
C8 . C9 . H91 . 118.0 no
C5 . C8 . C9 . 119.3(6) yes
C5 . C8 . H81 . 120.3 no
C9 . C8 . H81 . 120.2 no
C4 . C3 . C2 . 127.7(6) yes
C4 . C3 . H31 . 116.0 no
C2 . C3 . H31 . 116.2 no
C3 . C2 . O1 . 125.2(6) yes
C3 . C2 . C1 . 117.5(6) yes
O1 . C2 . C1 . 117.0(7) yes
Cu1 . O1 . C2 . 121.2(6) yes
C2 . C1 . H11 . 109.6 no
C2 . C1 . H12 . 110.8 no
H11 . C1 . H12 . 109.5 no
C2 . C1 . H13 . 108.0 no
H11 . C1 . H13 . 109.5 no
H12 . C1 . H13 . 109.5 no


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_MeOH_034_Lab
_database_code_depnum_ccdc_archive 'CCDC 1564967'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2020-06-09 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_audit_creation_date             2017-05-19
_audit_creation_method           CRYSTALS_ver_14.61_build_6236

_oxford_structure_analysis_title 'ST6093_0m in R-3'
_chemical_name_systematic        ?
_chemical_melting_point          ?

#end of refcif 
_cell_length_a                   26.6200(12)
_cell_length_b                   26.6200(12)
_cell_length_c                   7.7505(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4756.4(5)

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_space_group_name_Hall  '-R 3  '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3

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            9

# Given Formula = C24 H21.33 Cu1.33 N2.67 O5.33 
# Dc =      1.62 Fooo =   2388.00 Mu =     14.04 M =    517.18
# Found Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.22 FOOO =   1791.00 Mu =     10.53 M =    387.88

_chemical_formula_sum            'C18 H16 Cu1 N2 O4'
_chemical_formula_moiety         'C18 H16 Cu1 N2 O4'
_chemical_compound_source        ?
_chemical_formula_weight         387.88


_cell_measurement_reflns_used    2573
_cell_measurement_theta_min      3
_cell_measurement_theta_max      24
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1791
_exptl_absorpt_coefficient_mu    1.053

# Sheldrick geometric approximatio 0.81 0.90 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_T_max  0.90
_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      293
_diffrn_reflns_number            5412
_reflns_number_total             1318
_diffrn_reflns_av_R_equivalents  0.042
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 1318 
# Theoretical number of reflections is about 3492 


_diffrn_reflns_theta_min         3.167
_diffrn_reflns_theta_max         24.436
_diffrn_measured_fraction_theta_max 0.754

_diffrn_reflns_theta_full        18.327
_diffrn_measured_fraction_theta_full 0.827


_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_reflns_limit_h_min              -27
_reflns_limit_h_max              14
_reflns_limit_k_min              0
_reflns_limit_k_max              30
_reflns_limit_l_min              0
_reflns_limit_l_max              8

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.68
_refine_diff_density_max         0.60


# 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         1313
_refine_ls_number_restraints     126
_refine_ls_number_parameters     115
_oxford_refine_ls_R_factor_ref   0.0733
_refine_ls_wR_factor_ref         0.1656
_refine_ls_goodness_of_fit_ref   1.1296
_refine_ls_shift/su_max          0.0001389
_refine_ls_shift/su_mean         0.0000227


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1313
_refine_ls_R_factor_all          0.0733
_refine_ls_wR_factor_all         0.1656

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                1032
_refine_ls_R_factor_gt           0.0550
_refine_ls_wR_factor_gt          0.1503

# 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 +88.41P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# 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 0.8333 0.6667 0.6667 0.0346 1.0000 Uani S . . . . .
O2 O 0.76246(18) 0.63491(19) 0.5269(5) 0.0380 1.0000 Uani D U . . . .
C4 C 0.7135(2) 0.5934(3) 0.5743(7) 0.0383 1.0000 Uani D U . . . .
C5 C 0.6650(2) 0.5765(3) 0.4470(6) 0.0397 1.0000 Uani D U . . . .
C6 C 0.6778(3) 0.5953(3) 0.2776(7) 0.0541 1.0000 Uani D U . . . .
C7 C 0.6344(3) 0.5768(4) 0.1574(8) 0.0618 1.0000 Uani D U . . . .
N1 N 0.5790(2) 0.5404(2) 0.1937(6) 0.0442 1.0000 Uani D U . . . .
C9 C 0.5667(3) 0.5231(3) 0.3581(7) 0.0446 1.0000 Uani D U . . . .
C8 C 0.6078(2) 0.5400(3) 0.4867(7) 0.0457 1.0000 Uani D U . . . .
C3 C 0.7032(3) 0.5605(3) 0.7225(9) 0.0610 1.0000 Uani D U . . . .
C2 C 0.7466(2) 0.5617(3) 0.8295(8) 0.0516 1.0000 Uani D U . . . .
O1 O 0.7996(2) 0.5972(2) 0.8185(6) 0.0482 1.0000 Uani D U . . . .
C1 C 0.7272(4) 0.5156(4) 0.9667(12) 0.0872 1.0000 Uani D U . . . .
H61 H 0.7168 0.6212 0.2446 0.0629 1.0000 Uiso R . . . . .
H71 H 0.6443 0.5905 0.0424 0.0758 1.0000 Uiso R . . . . .
H91 H 0.5272 0.4985 0.3887 0.0539 1.0000 Uiso R . . . . .
H81 H 0.5967 0.5260 0.6011 0.0559 1.0000 Uiso R . . . . .
H31 H 0.6639 0.5349 0.7528 0.0737 1.0000 Uiso R . . . . .
H11 H 0.7568 0.5046 0.9862 0.1123 1.0000 Uiso R . . . . .
H12 H 0.7214 0.5320 1.0731 0.1123 1.0000 Uiso R . . . . .
H13 H 0.6906 0.4813 0.9334 0.1123 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.06691(4)
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 . N1 10_555 2.361(5) yes
Cu1 . N1 9_655 2.361(5) yes
Cu1 . O1 6_666 1.988(5) yes
Cu1 . O2 6_666 1.963(4) yes
Cu1 . O2 . 1.963(4) yes
Cu1 . O1 . 1.988(5) yes
O2 . C4 . 1.270(6) yes
C4 . C5 . 1.505(6) yes
C4 . C3 . 1.386(6) yes
C5 . C6 . 1.386(6) yes
C5 . C8 . 1.370(6) yes
C6 . C7 . 1.369(6) yes
C6 . H61 . 0.950 no
C7 . N1 . 1.328(6) yes
C7 . H71 . 0.950 no
N1 . C9 . 1.338(6) yes
C9 . C8 . 1.379(6) yes
C9 . H91 . 0.950 no
C8 . H81 . 0.950 no
C3 . C2 . 1.409(6) yes
C3 . H31 . 0.950 no
C2 . O1 . 1.249(6) yes
C2 . C1 . 1.508(7) yes
C1 . H11 . 0.980 no
C1 . H12 . 0.980 no
C1 . H13 . 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
N1 10_555 Cu1 . N1 9_655 179.995 yes
N1 10_555 Cu1 . O1 6_666 86.4(2) yes
N1 9_655 Cu1 . O1 6_666 93.7(2) yes
N1 10_555 Cu1 . O2 6_666 89.40(18) yes
N1 9_655 Cu1 . O2 6_666 90.60(18) yes
O1 6_666 Cu1 . O2 6_666 92.09(18) yes
N1 10_555 Cu1 . O2 . 90.60(18) yes
N1 9_655 Cu1 . O2 . 89.40(18) yes
O1 6_666 Cu1 . O2 . 87.91(18) yes
O2 6_666 Cu1 . O2 . 179.994 yes
N1 10_555 Cu1 . O1 . 93.6(2) yes
N1 9_655 Cu1 . O1 . 86.4(2) yes
O1 6_666 Cu1 . O1 . 179.994 yes
O2 6_666 Cu1 . O1 . 87.91(18) yes
O2 . Cu1 . O1 . 92.09(18) yes
Cu1 . O2 . C4 . 124.2(3) yes
O2 . C4 . C5 . 115.1(4) yes
O2 . C4 . C3 . 125.6(4) yes
C5 . C4 . C3 . 119.0(4) yes
C4 . C5 . C6 . 119.6(4) yes
C4 . C5 . C8 . 123.3(4) yes
C6 . C5 . C8 . 117.0(4) yes
C5 . C6 . C7 . 120.2(5) yes
C5 . C6 . H61 . 120.0 no
C7 . C6 . H61 . 119.8 no
C6 . C7 . N1 . 123.2(5) yes
C6 . C7 . H71 . 118.5 no
N1 . C7 . H71 . 118.3 no
Cu1 16_545 N1 . C7 . 127.5(4) yes
Cu1 16_545 N1 . C9 . 116.1(4) yes
C7 . N1 . C9 . 116.4(4) yes
N1 . C9 . C8 . 123.9(5) yes
N1 . C9 . H91 . 118.1 no
C8 . C9 . H91 . 118.0 no
C9 . C8 . C5 . 119.2(4) yes
C9 . C8 . H81 . 120.4 no
C5 . C8 . H81 . 120.4 no
C4 . C3 . C2 . 124.9(5) yes
C4 . C3 . H31 . 117.3 no
C2 . C3 . H31 . 117.8 no
C3 . C2 . O1 . 125.5(5) yes
C3 . C2 . C1 . 117.0(5) yes
O1 . C2 . C1 . 117.4(5) yes
C2 . O1 . Cu1 . 123.9(4) yes
C2 . C1 . H11 . 110.7 no
C2 . C1 . H12 . 107.3 no
H11 . C1 . H12 . 109.5 no
C2 . C1 . H13 . 110.4 no
H11 . C1 . H13 . 109.5 no
H12 . C1 . H13 . 109.4 no


# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 
# looking for PLATON_SQD.SQF 

# SQUEEZE RESULTS (Version =  60516) 
# Note: Data are Listed for all Voids in the P1 Unit Cell 
# i.e. Centre of Gravity, Solvent Accessible Volume, 
# Recovered number of Electrons in the Void and 
# Details about the Squeezed Material 
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 -0.004 414 133 ' '
2 0.333 0.667 0.696 418 132 ' '
3 0.667 0.333 0.363 418 132 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_MeOH_108_Lab
_database_code_depnum_ccdc_archive 'CCDC 1564969'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2020-06-09 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_audit_creation_date             2017-05-19
_audit_creation_method           CRYSTALS_ver_14.61_build_6236

_oxford_structure_analysis_title 'ST6099_0m in R-3'
_chemical_name_systematic        ?
_chemical_melting_point          ?

#end of refcif 
_cell_length_a                   25.7864(8)
_cell_length_b                   25.7864(8)
_cell_length_c                   7.7459(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4460.5(3)

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3

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            9

# Given Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.30 Fooo =   1791.00 Mu =     11.23 M =    387.88
# Found Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.30 FOOO =   1791.00 Mu =     11.23 M =    387.88

_chemical_formula_sum            'C18 H16 Cu1 N2 O4'
_chemical_formula_moiety         'C18 H16 Cu1 N2 O4'
_chemical_compound_source        ?
_chemical_formula_weight         387.88


_cell_measurement_reflns_used    2323
_cell_measurement_theta_min      3
_cell_measurement_theta_max      24
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1791
_exptl_absorpt_coefficient_mu    1.123

# Sheldrick geometric approximatio 0.80 0.89 
_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  0.89
_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            5087
_reflns_number_total             1240
_diffrn_reflns_av_R_equivalents  0.041
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 1240 
# Theoretical number of reflections is about 3282 


_diffrn_reflns_theta_min         3.201
_diffrn_reflns_theta_max         24.455
_diffrn_measured_fraction_theta_max 0.757

_diffrn_reflns_theta_full        18.341
_diffrn_measured_fraction_theta_full 0.828


_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_reflns_limit_h_min              -25
_reflns_limit_h_max              13
_reflns_limit_k_min              0
_reflns_limit_k_max              29
_reflns_limit_l_min              0
_reflns_limit_l_max              8

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.52
_refine_diff_density_max         0.50


# 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         1230
_refine_ls_number_restraints     126
_refine_ls_number_parameters     115
_oxford_refine_ls_R_factor_ref   0.0694
_refine_ls_wR_factor_ref         0.1613
_refine_ls_goodness_of_fit_ref   1.0139
_refine_ls_shift/su_max          0.0002091
_refine_ls_shift/su_mean         0.0000249


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1230
_refine_ls_R_factor_all          0.0694
_refine_ls_wR_factor_all         0.1613

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                980
_refine_ls_R_factor_gt           0.0514
_refine_ls_wR_factor_gt          0.1467

# 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) + ( 0.09P)² +32.77P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# 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 0.8333 0.6667 0.6667 0.0361 1.0000 Uani S . . . . .
O2 O 0.75905(16) 0.63474(17) 0.5323(4) 0.0454 1.0000 Uani D U . . . .
C4 C 0.7081(2) 0.5919(2) 0.5796(6) 0.0410 1.0000 Uani D U . . . .
C5 C 0.65889(19) 0.5741(2) 0.4497(5) 0.0398 1.0000 Uani D U . . . .
C6 C 0.6725(2) 0.5962(3) 0.2827(7) 0.0540 1.0000 Uani D U . . . .
C7 C 0.6291(2) 0.5761(3) 0.1585(7) 0.0579 1.0000 Uani D U . . . .
N1 N 0.57261(19) 0.5361(2) 0.1887(5) 0.0486 1.0000 Uani D U . . . .
C9 C 0.5591(2) 0.5154(3) 0.3507(6) 0.0526 1.0000 Uani D U . . . .
C8 C 0.5999(2) 0.5336(2) 0.4823(6) 0.0449 1.0000 Uani D U . . . .
C3 C 0.6958(2) 0.5591(3) 0.7310(7) 0.0575 1.0000 Uani D U . . . .
C2 C 0.7393(2) 0.5563(3) 0.8366(6) 0.0547 1.0000 Uani D U . . . .
O1 O 0.79464(17) 0.58880(19) 0.8216(5) 0.0570 1.0000 Uani D U . . . .
C1 C 0.7175(3) 0.5100(3) 0.9761(9) 0.0885 1.0000 Uani D U . . . .
H61 H 0.7125 0.6255 0.2542 0.0650 1.0000 Uiso R . . . . .
H71 H 0.6402 0.5916 0.0448 0.0692 1.0000 Uiso R . . . . .
H91 H 0.5188 0.4863 0.3757 0.0632 1.0000 Uiso R . . . . .
H81 H 0.5875 0.5182 0.5956 0.0536 1.0000 Uiso R . . . . .
H31 H 0.6552 0.5368 0.7666 0.0688 1.0000 Uiso R . . . . .
H11 H 0.7497 0.5027 1.0105 0.1044 1.0000 Uiso R . . . . .
H12 H 0.7048 0.5239 1.0762 0.1044 1.0000 Uiso R . . . . .
H13 H 0.6837 0.4727 0.9338 0.1044 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.06887(4)
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 . N1 9_655 2.183(4) yes
Cu1 . N1 10_555 2.183(4) yes
Cu1 . O1 6_666 2.113(4) yes
Cu1 . O2 6_666 1.963(3) yes
Cu1 . O2 . 1.963(3) yes
Cu1 . O1 . 2.113(4) yes
O2 . C4 . 1.276(5) yes
C4 . C5 . 1.500(5) yes
C4 . C3 . 1.387(6) yes
C5 . C6 . 1.386(6) yes
C5 . C8 . 1.371(6) yes
C6 . C7 . 1.367(6) yes
C6 . H61 . 0.950 no
C7 . N1 . 1.318(6) yes
C7 . H71 . 0.950 no
N1 . C9 . 1.340(5) yes
C9 . C8 . 1.368(6) yes
C9 . H91 . 0.950 no
C8 . H81 . 0.950 no
C3 . C2 . 1.419(6) yes
C3 . H31 . 0.950 no
C2 . O1 . 1.248(5) yes
C2 . C1 . 1.496(6) yes
C1 . H11 . 0.976 no
C1 . H12 . 0.977 no
C1 . H13 . 0.978 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
N1 9_655 Cu1 . N1 10_555 179.995 yes
N1 9_655 Cu1 . O1 6_666 94.09(16) yes
N1 10_555 Cu1 . O1 6_666 85.91(16) yes
N1 9_655 Cu1 . O2 6_666 90.10(15) yes
N1 10_555 Cu1 . O2 6_666 89.90(15) yes
O1 6_666 Cu1 . O2 6_666 90.26(15) yes
N1 9_655 Cu1 . O2 . 89.90(15) yes
N1 10_555 Cu1 . O2 . 90.10(15) yes
O1 6_666 Cu1 . O2 . 89.74(15) yes
O2 6_666 Cu1 . O2 . 179.994 yes
N1 9_655 Cu1 . O1 . 85.91(16) yes
N1 10_555 Cu1 . O1 . 94.09(16) yes
O1 6_666 Cu1 . O1 . 179.995 yes
O2 6_666 Cu1 . O1 . 89.74(15) yes
O2 . Cu1 . O1 . 90.26(15) yes
Cu1 . O2 . C4 . 125.3(3) yes
O2 . C4 . C5 . 114.8(3) yes
O2 . C4 . C3 . 126.4(4) yes
C5 . C4 . C3 . 118.7(4) yes
C4 . C5 . C6 . 119.9(4) yes
C4 . C5 . C8 . 123.8(4) yes
C6 . C5 . C8 . 116.2(4) yes
C5 . C6 . C7 . 120.6(4) yes
C5 . C6 . H61 . 119.7 no
C7 . C6 . H61 . 119.7 no
C6 . C7 . N1 . 123.2(4) yes
C6 . C7 . H71 . 118.4 no
N1 . C7 . H71 . 118.4 no
Cu1 16_545 N1 . C7 . 126.3(3) yes
Cu1 16_545 N1 . C9 . 117.4(3) yes
C7 . N1 . C9 . 116.3(4) yes
N1 . C9 . C8 . 124.0(4) yes
N1 . C9 . H91 . 118.0 no
C8 . C9 . H91 . 118.0 no
C5 . C8 . C9 . 119.6(4) yes
C5 . C8 . H81 . 120.2 no
C9 . C8 . H81 . 120.2 no
C4 . C3 . C2 . 125.0(4) yes
C4 . C3 . H31 . 117.5 no
C2 . C3 . H31 . 117.5 no
C3 . C2 . O1 . 125.4(4) yes
C3 . C2 . C1 . 117.8(4) yes
O1 . C2 . C1 . 116.8(4) yes
Cu1 . O1 . C2 . 122.0(3) yes
C2 . C1 . H11 . 109.5 no
C2 . C1 . H12 . 110.0 no
H11 . C1 . H12 . 109.2 no
C2 . C1 . H13 . 109.7 no
H11 . C1 . H13 . 109.2 no
H12 . C1 . H13 . 109.2 no



# 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 5 0 x .
-7 11 0 x .
2 3 2 x .
-18 12 6 x .
-7 17 0 x .
-17 11 2 x .
-1 2 3 x .
# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 
# looking for PLATON_SQD.SQF 

# SQUEEZE RESULTS (Version =  60516) 
# Note: Data are Listed for all Voids in the P1 Unit Cell 
# i.e. Centre of Gravity, Solvent Accessible Volume, 
# Recovered number of Electrons in the Void and 
# Details about the Squeezed Material 
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 -0.012 363 125 ' '
2 0.333 0.667 -0.175 367 125 ' '
3 0.667 0.333 0.084 367 125 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_FC70_156_Lab
_database_code_depnum_ccdc_archive 'CCDC 1564966'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2020-06-09 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_audit_creation_date             2016-06-10
_audit_creation_method           CRYSTALS_ver_14.61_build_5965

_oxford_structure_analysis_title 'st5140_0m in R-3'
_chemical_name_systematic        ?
_chemical_melting_point          ?

#end of refcif 
_cell_length_a                   25.2568(11)
_cell_length_b                   25.2568(11)
_cell_length_c                   7.7047(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4256.4(4)

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_space_group_name_Hall  '-R 3  '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3

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            9

# Given Formula = C10 H10 Cu1 N2 O10 
# Dc =      1.34 Fooo =   1737.00 Mu =     11.98 M =    381.74
# Found Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.36 FOOO =   1791.00 Mu =     11.77 M =    387.88

_chemical_formula_sum            'C18 H16 Cu1 N2 O4'
_chemical_formula_moiety         'C18 H16 Cu1 N2 O4'
_chemical_compound_source        ?
_chemical_formula_weight         387.88


_cell_measurement_reflns_used    1486
_cell_measurement_theta_min      3
_cell_measurement_theta_max      19
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1791
_exptl_absorpt_coefficient_mu    1.177

# Sheldrick geometric approximatio 0.79 0.89 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_T_max  0.89
_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_ambient_pressure         1560000
_diffrn_reflns_number            3936
_reflns_number_total             905
_diffrn_reflns_av_R_equivalents  0.092
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 905 
# Theoretical number of reflections is about 1978 


_diffrn_reflns_theta_min         3.234
_diffrn_reflns_theta_max         20.805
_diffrn_measured_fraction_theta_max 0.908

_diffrn_reflns_theta_full        15.604
_diffrn_measured_fraction_theta_full 0.933


_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_reflns_limit_h_min              -24
_reflns_limit_h_max              10
_reflns_limit_k_min              0
_reflns_limit_k_max              24
_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,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.18
_refine_diff_density_max         0.81


# 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>-3.0\s(I)
_refine_ls_number_reflns         902
_refine_ls_number_restraints     126
_refine_ls_number_parameters     115
_oxford_refine_ls_R_factor_ref   0.1380
_refine_ls_wR_factor_ref         0.2634
_refine_ls_goodness_of_fit_ref   1.0350
_refine_ls_shift/su_max          0.0000727
_refine_ls_shift/su_mean         0.0000101


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        902
_refine_ls_R_factor_all          0.1380
_refine_ls_wR_factor_all         0.2634

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                608
_refine_ls_R_factor_gt           0.0964
_refine_ls_wR_factor_gt          0.2125

# 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, 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: 
 8.17 10.1 2.73 
;

# 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 0.8333 0.6667 0.6667 0.0672 1.0000 Uani S . . . . .
O2 O 0.7570(4) 0.6338(4) 0.5328(12) 0.0755 1.0000 Uani D U . . . .
C4 C 0.7058(4) 0.5883(5) 0.5749(12) 0.0729 1.0000 Uani D U . . . .
C5 C 0.6567(4) 0.5706(5) 0.4417(11) 0.0682 1.0000 Uani D U . . . .
C6 C 0.6713(4) 0.5946(6) 0.2766(13) 0.0807 1.0000 Uani D U . . . .
C7 C 0.6273(5) 0.5742(7) 0.1500(13) 0.0926 1.0000 Uani D U . . . .
N1 N 0.5688(4) 0.5330(5) 0.1797(12) 0.0653 1.0000 Uani D U . . . .
C9 C 0.5549(4) 0.5123(6) 0.3425(13) 0.0788 1.0000 Uani D U . . . .
C8 C 0.5966(4) 0.5283(5) 0.4738(13) 0.0715 1.0000 Uani D U . . . .
C3 C 0.6929(4) 0.5532(6) 0.7219(15) 0.0893 1.0000 Uani D U . . . .
C2 C 0.7345(4) 0.5504(7) 0.8371(18) 0.0961 1.0000 Uani D U . . . .
O1 O 0.7914(4) 0.5838(5) 0.8288(13) 0.0833 1.0000 Uani D U . . . .
C1 C 0.7094(6) 0.5023(8) 0.978(2) 0.1080 1.0000 Uani D U . . . .
H61 H 0.7118 0.6257 0.2495 0.0954 1.0000 Uiso R . . . . .
H71 H 0.6387 0.5897 0.0355 0.1097 1.0000 Uiso R . . . . .
H91 H 0.5130 0.4861 0.3695 0.0749 1.0000 Uiso R . . . . .
H81 H 0.5839 0.5114 0.5866 0.0791 1.0000 Uiso R . . . . .
H31 H 0.6508 0.5282 0.7498 0.1029 1.0000 Uiso R . . . . .
H11 H 0.7432 0.5050 1.0471 0.1340 1.0000 Uiso R . . . . .
H12 H 0.6820 0.5091 1.0526 0.1340 1.0000 Uiso R . . . . .
H13 H 0.6867 0.4616 0.9250 0.1340 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.06770(7)
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 6_666 2.201(10) yes
Cu1 . N1 9_655 2.046(8) yes
Cu1 . N1 10_555 2.046(8) yes
Cu1 . O2 6_666 1.966(8) yes
Cu1 . O2 . 1.966(8) yes
Cu1 . O1 . 2.201(10) yes
O2 . C4 . 1.270(7) yes
C4 . C5 . 1.495(7) yes
C4 . C3 . 1.373(8) yes
C5 . C6 . 1.378(8) yes
C5 . C8 . 1.374(8) yes
C6 . C7 . 1.371(8) yes
C6 . H61 . 0.950 no
C7 . N1 . 1.334(8) yes
C7 . H71 . 0.950 no
N1 . C9 . 1.336(8) yes
C9 . C8 . 1.366(8) yes
C9 . H91 . 0.950 no
C8 . H81 . 0.950 no
C3 . C2 . 1.405(8) yes
C3 . H31 . 0.950 no
C2 . O1 . 1.252(8) yes
C2 . C1 . 1.510(8) yes
C1 . H11 . 0.980 no
C1 . H12 . 0.980 no
C1 . H13 . 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
O1 6_666 Cu1 . N1 9_655 94.2(4) yes
O1 6_666 Cu1 . N1 10_555 85.8(4) yes
N1 9_655 Cu1 . N1 10_555 179.994 yes
O1 6_666 Cu1 . O2 6_666 89.5(3) yes
N1 9_655 Cu1 . O2 6_666 89.3(4) yes
N1 10_555 Cu1 . O2 6_666 90.7(4) yes
O1 6_666 Cu1 . O2 . 90.5(3) yes
N1 9_655 Cu1 . O2 . 90.7(4) yes
N1 10_555 Cu1 . O2 . 89.3(4) yes
O2 6_666 Cu1 . O2 . 179.994 yes
O1 6_666 Cu1 . O1 . 179.995 yes
N1 9_655 Cu1 . O1 . 85.8(4) yes
N1 10_555 Cu1 . O1 . 94.2(4) yes
O2 6_666 Cu1 . O1 . 90.5(3) yes
O2 . Cu1 . O1 . 89.5(3) yes
Cu1 . O2 . C4 . 126.1(6) yes
O2 . C4 . C5 . 114.4(5) yes
O2 . C4 . C3 . 126.8(6) yes
C5 . C4 . C3 . 118.7(5) yes
C4 . C5 . C6 . 120.2(5) yes
C4 . C5 . C8 . 122.5(5) yes
C6 . C5 . C8 . 117.2(5) yes
C5 . C6 . C7 . 120.2(6) yes
C5 . C6 . H61 . 120.5 no
C7 . C6 . H61 . 119.4 no
C6 . C7 . N1 . 123.0(6) yes
C6 . C7 . H71 . 118.9 no
N1 . C7 . H71 . 118.1 no
C7 . N1 . Cu1 16_545 125.8(6) yes
C7 . N1 . C9 . 116.0(6) yes
Cu1 16_545 N1 . C9 . 118.2(6) yes
N1 . C9 . C8 . 124.5(6) yes
N1 . C9 . H91 . 117.5 no
C8 . C9 . H91 . 118.0 no
C5 . C8 . C9 . 119.0(6) yes
C5 . C8 . H81 . 120.5 no
C9 . C8 . H81 . 120.5 no
C4 . C3 . C2 . 127.8(6) yes
C4 . C3 . H31 . 116.2 no
C2 . C3 . H31 . 116.0 no
C3 . C2 . O1 . 124.6(6) yes
C3 . C2 . C1 . 118.1(6) yes
O1 . C2 . C1 . 117.3(6) yes
Cu1 . O1 . C2 . 121.0(6) yes
C2 . C1 . H11 . 109.5 no
C2 . C1 . H12 . 109.3 no
H11 . C1 . H12 . 109.5 no
C2 . C1 . H13 . 109.6 no
H11 . C1 . H13 . 109.5 no
H12 . C1 . H13 . 109.5 no


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_MeOH_071_Lab
_database_code_depnum_ccdc_archive 'CCDC 1564968'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2020-06-09 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_audit_creation_date             2017-05-19
_audit_creation_method           CRYSTALS_ver_14.61_build_6236

_oxford_structure_analysis_title 'ST6098_0m in R-3'
_chemical_name_systematic        ?
_chemical_melting_point          ?

#end of refcif 
_cell_length_a                   26.1591(14)
_cell_length_b                   26.1591(14)
_cell_length_c                   7.7544(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4595.4(5)

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_space_group_name_Hall  '-R 3 '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3

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            9

# Given Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.26 Fooo =   1791.00 Mu =     10.90 M =    387.88
# Found Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.26 FOOO =   1791.00 Mu =     10.90 M =    387.88

_chemical_formula_sum            'C18 H16 Cu1 N2 O4'
_chemical_formula_moiety         'C18 H16 Cu1 N2 O4'
_chemical_compound_source        ?
_chemical_formula_weight         387.88


_cell_measurement_reflns_used    2491
_cell_measurement_theta_min      3
_cell_measurement_theta_max      24
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1791
_exptl_absorpt_coefficient_mu    1.090

# Sheldrick geometric approximatio 0.80 0.90 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.53
_exptl_absorpt_correction_T_max  0.90
_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            5061
_reflns_number_total             1255
_diffrn_reflns_av_R_equivalents  0.042
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 1255 
# Theoretical number of reflections is about 3372 


_diffrn_reflns_theta_min         3.184
_diffrn_reflns_theta_max         24.431
_diffrn_measured_fraction_theta_max 0.743

_diffrn_reflns_theta_full        18.323
_diffrn_measured_fraction_theta_full 0.837


_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_reflns_limit_h_min              -26
_reflns_limit_h_max              13
_reflns_limit_k_min              0
_reflns_limit_k_max              30
_reflns_limit_l_min              0
_reflns_limit_l_max              8

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.61
_refine_diff_density_max         0.58


# 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         1247
_refine_ls_number_restraints     126
_refine_ls_number_parameters     115
_oxford_refine_ls_R_factor_ref   0.0744
_refine_ls_wR_factor_ref         0.1817
_refine_ls_goodness_of_fit_ref   0.9837
_refine_ls_shift/su_max          0.0001931
_refine_ls_shift/su_mean         0.0000224


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1247
_refine_ls_R_factor_all          0.0744
_refine_ls_wR_factor_all         0.1817

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                973
_refine_ls_R_factor_gt           0.0559
_refine_ls_wR_factor_gt          0.1579

# 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) + ( 0.11P)² +46.46P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# 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 0.8333 0.6667 0.6667 0.0354 1.0000 Uani S . . . . .
O2 O 0.76097(17) 0.63492(18) 0.5297(5) 0.0432 1.0000 Uani D U . . . .
C4 C 0.7108(2) 0.5932(2) 0.5773(6) 0.0415 1.0000 Uani D U . . . .
C5 C 0.6620(2) 0.5760(2) 0.4501(6) 0.0382 1.0000 Uani D U . . . .
C6 C 0.6752(2) 0.5965(3) 0.2823(7) 0.0566 1.0000 Uani D U . . . .
C7 C 0.6324(3) 0.5769(3) 0.1591(7) 0.0616 1.0000 Uani D U . . . .
N1 N 0.5761(2) 0.5390(2) 0.1917(6) 0.0511 1.0000 Uani D U . . . .
C9 C 0.5626(2) 0.5191(3) 0.3548(7) 0.0525 1.0000 Uani D U . . . .
C8 C 0.6041(2) 0.5369(3) 0.4850(6) 0.0489 1.0000 Uani D U . . . .
C3 C 0.6997(2) 0.5606(3) 0.7275(7) 0.0591 1.0000 Uani D U . . . .
C2 C 0.7430(2) 0.5588(3) 0.8323(7) 0.0542 1.0000 Uani D U . . . .
O1 O 0.79756(19) 0.5931(2) 0.8187(5) 0.0536 1.0000 Uani D U . . . .
C1 C 0.7227(3) 0.5127(3) 0.9705(10) 0.0840 1.0000 Uani D U . . . .
H61 H 0.7144 0.6231 0.2501 0.0716 1.0000 Uiso R . . . . .
H71 H 0.6424 0.5906 0.0439 0.0733 1.0000 Uiso R . . . . .
H91 H 0.5229 0.4926 0.3828 0.0588 1.0000 Uiso R . . . . .
H81 H 0.5923 0.5234 0.5996 0.0556 1.0000 Uiso R . . . . .
H31 H 0.6601 0.5359 0.7598 0.0741 1.0000 Uiso R . . . . .
H11 H 0.7552 0.5067 1.0058 0.1103 1.0000 Uiso R . . . . .
H12 H 0.7091 0.5257 1.0703 0.1103 1.0000 Uiso R . . . . .
H13 H 0.6900 0.4755 0.9270 0.1103 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.06758(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 . N1 10_555 2.277(4) yes
Cu1 . N1 9_655 2.277(4) yes
Cu1 . O1 6_666 2.042(4) yes
Cu1 . O2 6_666 1.957(4) yes
Cu1 . O2 . 1.957(4) yes
Cu1 . O1 . 2.042(4) yes
O2 . C4 . 1.271(5) yes
C4 . C5 . 1.494(6) yes
C4 . C3 . 1.385(6) yes
C5 . C6 . 1.384(6) yes
C5 . C8 . 1.367(6) yes
C6 . C7 . 1.363(6) yes
C6 . H61 . 0.940 no
C7 . N1 . 1.324(6) yes
C7 . H71 . 0.949 no
N1 . C9 . 1.346(6) yes
C9 . C8 . 1.381(6) yes
C9 . H91 . 0.940 no
C8 . H81 . 0.949 no
C3 . C2 . 1.415(6) yes
C3 . H31 . 0.940 no
C2 . O1 . 1.253(5) yes
C2 . C1 . 1.498(6) yes
C1 . H11 . 0.979 no
C1 . H12 . 0.980 no
C1 . H13 . 0.981 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
N1 10_555 Cu1 . N1 9_655 179.995 yes
N1 10_555 Cu1 . O1 6_666 86.20(18) yes
N1 9_655 Cu1 . O1 6_666 93.80(18) yes
N1 10_555 Cu1 . O2 6_666 89.49(17) yes
N1 9_655 Cu1 . O2 6_666 90.51(17) yes
O1 6_666 Cu1 . O2 6_666 91.33(16) yes
N1 10_555 Cu1 . O2 . 90.51(17) yes
N1 9_655 Cu1 . O2 . 89.49(17) yes
O1 6_666 Cu1 . O2 . 88.67(16) yes
O2 6_666 Cu1 . O2 . 179.994 yes
N1 10_555 Cu1 . O1 . 93.80(18) yes
N1 9_655 Cu1 . O1 . 86.20(18) yes
O1 6_666 Cu1 . O1 . 179.994 yes
O2 6_666 Cu1 . O1 . 88.67(16) yes
O2 . Cu1 . O1 . 91.33(16) yes
Cu1 . O2 . C4 . 124.8(3) yes
O2 . C4 . C5 . 115.2(4) yes
O2 . C4 . C3 . 125.6(4) yes
C5 . C4 . C3 . 119.0(4) yes
C4 . C5 . C6 . 119.6(4) yes
C4 . C5 . C8 . 123.8(4) yes
C6 . C5 . C8 . 116.4(4) yes
C5 . C6 . C7 . 121.0(4) yes
C5 . C6 . H61 . 120.3 no
C7 . C6 . H61 . 118.6 no
C6 . C7 . N1 . 123.0(4) yes
C6 . C7 . H71 . 119.8 no
N1 . C7 . H71 . 117.2 no
Cu1 16_545 N1 . C7 . 127.3(3) yes
Cu1 16_545 N1 . C9 . 116.0(3) yes
C7 . N1 . C9 . 116.7(4) yes
N1 . C9 . C8 . 123.0(4) yes
N1 . C9 . H91 . 118.8 no
C8 . C9 . H91 . 118.1 no
C9 . C8 . C5 . 119.9(4) yes
C9 . C8 . H81 . 120.3 no
C5 . C8 . H81 . 119.7 no
C4 . C3 . C2 . 125.3(4) yes
C4 . C3 . H31 . 117.9 no
C2 . C3 . H31 . 116.7 no
C3 . C2 . O1 . 124.9(4) yes
C3 . C2 . C1 . 118.0(4) yes
O1 . C2 . C1 . 117.1(4) yes
C2 . O1 . Cu1 . 123.0(3) yes
C2 . C1 . H11 . 110.0 no
C2 . C1 . H12 . 109.3 no
H11 . C1 . H12 . 109.3 no
C2 . C1 . H13 . 109.6 no
H11 . C1 . H13 . 109.5 no
H12 . C1 . H13 . 109.2 no



# 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 14 0 x .
-6 16 2 x .
-5 3 1 x .
-10 22 1 x .
-18 12 6 x .
# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 
# looking for PLATON_SQD.SQF 

# SQUEEZE RESULTS (Version =  60516) 
# Note: Data are Listed for all Voids in the P1 Unit Cell 
# i.e. Centre of Gravity, Solvent Accessible Volume, 
# Recovered number of Electrons in the Void and 
# Details about the Squeezed Material 
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 -0.004 390 140 ' '
2 0.333 0.667 0.688 394 140 ' '
3 0.667 0.333 0.355 394 140 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_MeOH_177_Lab
_database_code_depnum_ccdc_archive 'CCDC 1564972'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2020-06-09 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_audit_creation_date             2017-05-19
_audit_creation_method           CRYSTALS_ver_14.61_build_6236

_oxford_structure_analysis_title 'ST6106_0m in R-3'
_chemical_name_systematic        ?
_chemical_melting_point          ?

#end of refcif 
_cell_length_a                   25.3023(7)
_cell_length_b                   25.3023(7)
_cell_length_c                   7.7337(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4287.8(3)

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3

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            9

# Given Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.35 Fooo =   1791.00 Mu =     11.68 M =    387.88
# Found Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.35 FOOO =   1791.00 Mu =     11.68 M =    387.88

_chemical_formula_sum            'C18 H16 Cu1 N2 O4'
_chemical_formula_moiety         'C18 H16 Cu1 N2 O4'
_chemical_compound_source        ?
_chemical_formula_weight         387.88


_cell_measurement_reflns_used    2594
_cell_measurement_theta_min      3
_cell_measurement_theta_max      24
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1791
_exptl_absorpt_coefficient_mu    1.168

# Sheldrick geometric approximatio 0.79 0.89 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_T_max  0.89
_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            4844
_reflns_number_total             1180
_diffrn_reflns_av_R_equivalents  0.039
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 1180 
# Theoretical number of reflections is about 3152 


_diffrn_reflns_theta_min         3.224
_diffrn_reflns_theta_max         24.448
_diffrn_measured_fraction_theta_max 0.750

_diffrn_reflns_theta_full        18.336
_diffrn_measured_fraction_theta_full 0.824


_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_reflns_limit_h_min              -26
_reflns_limit_h_max              12
_reflns_limit_k_min              0
_reflns_limit_k_max              29
_reflns_limit_l_min              0
_reflns_limit_l_max              8

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.40
_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         1177
_refine_ls_number_restraints     126
_refine_ls_number_parameters     115
_oxford_refine_ls_R_factor_ref   0.0576
_refine_ls_wR_factor_ref         0.1211
_refine_ls_goodness_of_fit_ref   0.8986
_refine_ls_shift/su_max          0.0001709
_refine_ls_shift/su_mean         0.0000270


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1177
_refine_ls_R_factor_all          0.0576
_refine_ls_wR_factor_all         0.1211

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                977
_refine_ls_R_factor_gt           0.0459
_refine_ls_wR_factor_gt          0.1112

# 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) + ( 0.05P)² +53.23P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# 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 0.8333 0.6667 0.6667 0.0292 1.0000 Uani S . . . . .
O2 O 0.75704(13) 0.63486(15) 0.5362(4) 0.0360 1.0000 Uani D U . . . .
C4 C 0.70503(17) 0.59128(19) 0.5835(5) 0.0320 1.0000 Uani D U . . . .
C5 C 0.65572(17) 0.57301(19) 0.4518(5) 0.0297 1.0000 Uani D U . . . .
C6 C 0.6705(2) 0.5976(2) 0.2858(6) 0.0437 1.0000 Uani D U . . . .
C7 C 0.6265(2) 0.5764(2) 0.1589(6) 0.0433 1.0000 Uani D U . . . .
N1 N 0.56938(16) 0.53332(17) 0.1858(4) 0.0353 1.0000 Uani D U . . . .
C9 C 0.5552(2) 0.5112(2) 0.3466(5) 0.0426 1.0000 Uani D U . . . .
C8 C 0.59562(19) 0.5296(2) 0.4809(5) 0.0376 1.0000 Uani D U . . . .
C3 C 0.6920(2) 0.5580(2) 0.7346(6) 0.0445 1.0000 Uani D U . . . .
C2 C 0.7349(2) 0.5544(2) 0.8432(6) 0.0454 1.0000 Uani D U . . . .
O1 O 0.79138(15) 0.58404(16) 0.8243(4) 0.0440 1.0000 Uani D U . . . .
C1 C 0.7106(3) 0.5074(3) 0.9844(8) 0.0773 1.0000 Uani D U . . . .
H61 H 0.7111 0.6286 0.2606 0.0518 1.0000 Uiso R . . . . .
H71 H 0.6379 0.5942 0.0471 0.0529 1.0000 Uiso R . . . . .
H91 H 0.5142 0.4804 0.3685 0.0505 1.0000 Uiso R . . . . .
H81 H 0.5823 0.5127 0.5929 0.0465 1.0000 Uiso R . . . . .
H31 H 0.6504 0.5355 0.7687 0.0597 1.0000 Uiso R . . . . .
H11 H 0.7443 0.5088 1.0506 0.0931 1.0000 Uiso R . . . . .
H12 H 0.6852 0.5159 1.0619 0.0931 1.0000 Uiso R . . . . .
H13 H 0.6860 0.4665 0.9347 0.0931 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.07241(4)
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 6_666 2.183(3) yes
Cu1 . N1 9_655 2.092(3) yes
Cu1 . N1 10_555 2.092(3) yes
Cu1 . O2 6_666 1.959(3) yes
Cu1 . O2 . 1.959(3) yes
Cu1 . O1 . 2.183(3) yes
O2 . C4 . 1.277(4) yes
C4 . C5 . 1.494(5) yes
C4 . C3 . 1.380(5) yes
C5 . C6 . 1.393(5) yes
C5 . C8 . 1.378(5) yes
C6 . C7 . 1.377(5) yes
C6 . H61 . 0.950 no
C7 . N1 . 1.321(5) yes
C7 . H71 . 0.950 no
N1 . C9 . 1.337(5) yes
C9 . C8 . 1.367(5) yes
C9 . H91 . 0.950 no
C8 . H81 . 0.950 no
C3 . C2 . 1.410(5) yes
C3 . H31 . 0.950 no
C2 . O1 . 1.248(5) yes
C2 . C1 . 1.501(6) yes
C1 . H11 . 0.979 no
C1 . H12 . 0.979 no
C1 . H13 . 0.981 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 6_666 Cu1 . N1 9_655 94.30(14) yes
O1 6_666 Cu1 . N1 10_555 85.70(14) yes
N1 9_655 Cu1 . N1 10_555 179.995 yes
O1 6_666 Cu1 . O2 6_666 89.24(13) yes
N1 9_655 Cu1 . O2 6_666 89.79(13) yes
N1 10_555 Cu1 . O2 6_666 90.21(13) yes
O1 6_666 Cu1 . O2 . 90.76(13) yes
N1 9_655 Cu1 . O2 . 90.21(13) yes
N1 10_555 Cu1 . O2 . 89.79(13) yes
O2 6_666 Cu1 . O2 . 179.994 yes
O1 6_666 Cu1 . O1 . 179.995 yes
N1 9_655 Cu1 . O1 . 85.70(14) yes
N1 10_555 Cu1 . O1 . 94.30(14) yes
O2 6_666 Cu1 . O1 . 90.76(13) yes
O2 . Cu1 . O1 . 89.24(13) yes
Cu1 . O2 . C4 . 125.8(3) yes
O2 . C4 . C5 . 114.3(3) yes
O2 . C4 . C3 . 126.7(3) yes
C5 . C4 . C3 . 118.8(3) yes
C4 . C5 . C6 . 119.6(3) yes
C4 . C5 . C8 . 123.6(3) yes
C6 . C5 . C8 . 116.7(3) yes
C5 . C6 . C7 . 119.9(4) yes
C5 . C6 . H61 . 119.8 no
C7 . C6 . H61 . 120.3 no
C6 . C7 . N1 . 123.2(4) yes
C6 . C7 . H71 . 118.0 no
N1 . C7 . H71 . 118.8 no
C7 . N1 . Cu1 16_545 125.2(3) yes
C7 . N1 . C9 . 116.5(3) yes
Cu1 16_545 N1 . C9 . 118.3(3) yes
N1 . C9 . C8 . 124.4(4) yes
N1 . C9 . H91 . 117.7 no
C8 . C9 . H91 . 117.9 no
C5 . C8 . C9 . 119.1(3) yes
C5 . C8 . H81 . 120.6 no
C9 . C8 . H81 . 120.2 no
C4 . C3 . C2 . 126.0(4) yes
C4 . C3 . H31 . 117.1 no
C2 . C3 . H31 . 116.9 no
C3 . C2 . O1 . 125.4(4) yes
C3 . C2 . C1 . 117.5(4) yes
O1 . C2 . C1 . 116.9(4) yes
Cu1 . O1 . C2 . 120.2(3) yes
C2 . C1 . H11 . 110.4 no
C2 . C1 . H12 . 108.9 no
H11 . C1 . H12 . 109.1 no
C2 . C1 . H13 . 110.1 no
H11 . C1 . H13 . 109.1 no
H12 . C1 . H13 . 109.2 no


# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 
# looking for PLATON_SQD.SQF 

# SQUEEZE RESULTS (Version =  60516) 
# Note: Data are Listed for all Voids in the P1 Unit Cell 
# i.e. Centre of Gravity, Solvent Accessible Volume, 
# Recovered number of Electrons in the Void and 
# Details about the Squeezed Material 
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 -0.012 342 115 ' '
2 0.333 0.667 -0.179 345 115 ' '
3 0.667 0.333 0.102 346 115 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CuPyrIII
_database_code_depnum_ccdc_archive 'CCDC 2008843'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2020-06-09 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_audit_creation_date             2014-12-22
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C54 H48 Cu3 N6 O12, C4 H10 O'
_chemical_formula_sum            'C58 H58 Cu3 N6 O13'
_chemical_formula_weight         1237.72
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N8 O20 Cu Gd'
_chemical_oxdiff_usercomment     '@ 200 K PC1469'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.7799(3)
_cell_length_b                   15.1586(9)
_cell_length_c                   15.4901(9)
_cell_angle_alpha                116.604(6)
_cell_angle_beta                 100.395(4)
_cell_angle_gamma                98.422(4)
_cell_volume                     1551.99(15)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9584
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      76.4050
_cell_measurement_theta_min      5.7750
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.717
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rod
_exptl_crystal_F_000             639
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'The material was recrystallised from diethyl ether by slow evaporation'
_exptl_crystal_size_max          0.1991
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.0449
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_Laue_measured_fraction_full 0.925
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20345
_diffrn_reflns_point_group_measured_fraction_full 0.925
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        66.000
_diffrn_reflns_theta_max         76.540
_diffrn_reflns_theta_min         3.322
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -37.00   84.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -120.0000 121

#__ type_ start__ end____ width___ exp.time_
  2 omega  -95.00  -34.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  -30.0000 61

#__ type_ start__ end____ width___ exp.time_
  3 omega  -37.00   84.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 121

#__ type_ start__ end____ width___ exp.time_
  4 omega  -50.00   25.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000   38.0000  -30.0000 75

#__ type_ start__ end____ width___ exp.time_
  5 omega  -96.00   -2.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000  125.0000 -180.0000 94

#__ type_ start__ end____ width___ exp.time_
  6 omega -148.00  -79.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000  -99.0000   30.0000 69

#__ type_ start__ end____ width___ exp.time_
  7 omega  -50.00   25.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000   38.0000   90.0000 75

#__ type_ start__ end____ width___ exp.time_
  8 omega -143.00  -22.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000  -38.0000  -60.0000 121

#__ type_ start__ end____ width___ exp.time_
  9 omega   94.00  143.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       59.0000  125.0000 -120.0000 49

#__ type_ start__ end____ width___ exp.time_
 10 omega    1.00  106.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       59.0000  -99.0000  -30.0000 105

#__ type_ start__ end____ width___ exp.time_
 11 omega   34.00   93.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -38.0000   60.0000 59

#__ type_ start__ end____ width___ exp.time_
 12 omega  100.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  111.0000 -180.0000 78

#__ type_ start__ end____ width___ exp.time_
 13 omega  100.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  111.0000   30.0000 78

#__ type_ start__ end____ width___ exp.time_
 14 omega   57.00  150.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  178.0000  -60.0000 93

#__ type_ start__ end____ width___ exp.time_
 15 omega   32.00  116.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000 -111.0000  -90.0000 84

#__ type_ start__ end____ width___ exp.time_
 16 omega   32.00  116.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000 -111.0000   30.0000 84

#__ type_ start__ end____ width___ exp.time_
 17 omega   57.00  150.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  178.0000 -180.0000 93

#__ type_ start__ end____ width___ exp.time_
 18 omega  100.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  111.0000  150.0000 78

#__ type_ start__ end____ width___ exp.time_
 19 omega   32.00  116.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000 -111.0000 -120.0000 84

#__ type_ start__ end____ width___ exp.time_
 20 omega  100.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  111.0000   90.0000 78

#__ type_ start__ end____ width___ exp.time_
 21 omega   81.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000   63.0000  150.0000 97

#__ type_ start__ end____ width___ exp.time_
 22 omega   33.00  155.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -63.0000   60.0000 122

#__ type_ start__ end____ width___ exp.time_
 23 omega   34.00   93.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -38.0000 -150.0000 59

#__ type_ start__ end____ width___ exp.time_
 24 omega   34.00   93.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -38.0000  150.0000 59

#__ type_ start__ end____ width___ exp.time_
 25 omega   32.00  116.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000 -111.0000  -30.0000 84

#__ type_ start__ end____ width___ exp.time_
 26 omega   32.00  116.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000 -111.0000  120.0000 84

#__ type_ start__ end____ width___ exp.time_
 27 omega   63.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000   25.0000  -90.0000 115

#__ type_ start__ end____ width___ exp.time_
 28 omega   34.00   93.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -38.0000  -60.0000 59

#__ type_ start__ end____ width___ exp.time_
 29 omega   32.00  116.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000 -111.0000  150.0000 84

#__ type_ start__ end____ width___ exp.time_
 30 omega    1.00   47.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000   60.0000 46

#__ type_ start__ end____ width___ exp.time_
 31 omega    1.00   47.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000   30.0000 46

#__ type_ start__ end____ width___ exp.time_
 32 omega  -39.00   92.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000    0.0000 131

#__ type_ start__ end____ width___ exp.time_
 33 omega -151.00  -20.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000  -77.0000  -90.0000 131

#__ type_ start__ end____ width___ exp.time_
 34 omega -143.00  -22.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000  -57.0000 -180.0000 121

#__ type_ start__ end____ width___ exp.time_
 35 omega -143.00  -22.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000  -57.0000  120.0000 121

#__ type_ start__ end____ width___ exp.time_
 36 omega -151.00  -20.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000  -77.0000   60.0000 131

#__ type_ start__ end____ width___ exp.time_
 37 omega -151.00  -20.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000  -77.0000    0.0000 131

#__ type_ start__ end____ width___ exp.time_
 38 omega -143.00  -22.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000  -57.0000   60.0000 121

#__ type_ start__ end____ width___ exp.time_
 39 omega -151.00  -75.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000  -77.0000 -150.0000 76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent Technologies SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0305141000
_diffrn_orient_matrix_UB_12      0.0679958000
_diffrn_orient_matrix_UB_13      -0.0483282000
_diffrn_orient_matrix_UB_21      -0.0709540000
_diffrn_orient_matrix_UB_22      -0.0957698000
_diffrn_orient_matrix_UB_23      -0.1046274000
_diffrn_orient_matrix_UB_31      -0.1935574000
_diffrn_orient_matrix_UB_32      -0.0083973000
_diffrn_orient_matrix_UB_33      0.0112142000
loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.5790 12952 12013
2 0.4210 0 12013

_diffrn_oxdiff_twin_integration_method simultaneous
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4475
_reflns_number_total             5968
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.505
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.155
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         5968
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0610
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1433P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1809
_refine_ls_wR_factor_ref         0.1977
_refine_special_details          
;
Several crystals were examined, each gave a diffraction pattern which was split or twinned in appearance, despite good appearance of all crystals on a polarizing microscope. Data were measured at 200 K in an attempt to alleviate this problem which was thought to be caused by flash cooling at lower temperatures. The program CrysAlisPro was used to identify two different split crystal domains corresponding to a 180 degree rotation about the [0 -0.71 0.71] reciprocal lattice direction. The two components were integrated separately and only those reflections corresponding to component 1 were used in the output reflection file, which explains the completeness of < 100 pc. Refinement of the model against a multicomponenet reflection file gives an unstable result. Refinement of the diethyl ether molecule is significantly improved when the the occupancy of the molecule is fixed at 0.5 (free refinement gives occupancy of about 0.55) and the molecule is assumed to be disordered about a crystallographic inversion centre. All of the copper centres lie on crystallographic inversion centres.


#-------------------------------------------------------------------------------

INTENSITY STATISTICS FOR DATASET # 1  eb4306.hkl

 Resolution   #Data #Theory %Complete Redundancy Mean I Mean I/s Rmerge  Rsigma

  Inf - 3.08      90    111     81.1     4.06   1001.15  114.61  0.0555  0.0074
 3.08 - 2.11     211    244     86.5     6.00    536.53   82.26  0.0549  0.0083
 2.11 - 1.67     298    342     87.1     3.87    373.89   52.96  0.0618  0.0142
 1.67 - 1.47     298    330     90.3     3.55    233.78   30.50  0.0572  0.0240
 1.47 - 1.33     322    351     91.7     3.32    203.83   24.98  0.0628  0.0302
 1.33 - 1.24     292    317     92.1     3.02    175.10   20.34  0.0811  0.0386
 1.24 - 1.17     313    335     93.4     3.31     77.84   12.46  0.0997  0.0720
 1.17 - 1.12     266    283     94.0     5.06    113.37   23.41  0.1016  0.0357
 1.12 - 1.07     326    342     95.3     5.45     81.39   21.27  0.0940  0.0447
 1.07 - 1.03     310    321     96.6     4.44     60.87   15.20  0.1101  0.0622
 1.03 - 0.99     341    371     91.9     2.64     62.14   13.89  0.0710  0.0651
 0.99 - 0.96     291    314     92.7     2.66     59.58   14.18  0.0657  0.0661
 0.96 - 0.94     245    260     94.2     2.80     48.35   12.77  0.0903  0.0750
 0.94 - 0.91     361    389     92.8     2.51     39.43   10.83  0.0721  0.0897
 0.91 - 0.89     272    289     94.1     2.60     32.89   10.05  0.0935  0.0965
 0.89 - 0.87     302    325     92.9     2.27     31.08    9.36  0.0946  0.1026
 0.87 - 0.85     347    362     95.9     2.38     26.40    8.92  0.1142  0.1099
 0.85 - 0.84     182    194     93.8     2.28     25.51    8.76  0.1034  0.1070
 0.84 - 0.82     403    427     94.4     2.00     19.41    7.42  0.1047  0.1353
 0.82 - 0.81     200    207     96.6     1.86     16.38    6.45  0.1217  0.1516
 0.81 - 0.79     298    414     72.0     1.04     14.66    5.53  0.1109  0.1745
#------------------------------------------------------------------------------
 0.89 - 0.79    1732   1929     89.8     1.93     22.32    7.76  0.1057  0.1237
  Inf - 0.79    5968   6528     91.4     3.12    119.52   20.17  0.0683  0.0341

Merged [A],  lowest resolution = 13.30 Angstroms                              

#-------------------------------------------------------------------------------



;

_vrf_PLAT341_eb4306              
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0068 Ang.  
RESPONSE: Please see _refine_special_details.
;


_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 O7, C28, C30, C29, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: O7(0.5) C28(0.5) H28A(0.5) H28B(0.5) C30(0.5) H30A(0.5) H30B(0.5)
 C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C30(H30A,H30B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C10(H10), C11(H11), C13(H13),
 C14(H14), C16(H16), C19(H19), C20(H20), C22(H22), C23(H23), C25(H25)
4.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C18(H18A,H18B,H18C), C27(H27A,H27B,H27C), C29(H29A,H29B,
 H29C), C31(H31A,H31B,H31C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.5000 1.0000 1.0000 0.0304(2) Uani 1 2 d S T P . .
Cu2 Cu -0.5000 0.5000 0.5000 0.0301(2) Uani 1 2 d S T P . .
Cu3 Cu -1.0000 0.5000 1.0000 0.0286(2) Uani 1 2 d S T P . .
O1 O 0.3909(4) 1.11057(19) 1.0055(2) 0.0339(5) Uani 1 1 d . . . . .
O2 O 0.6116(4) 0.9971(2) 0.8932(2) 0.0393(6) Uani 1 1 d . . . . .
O3 O -0.2896(3) 0.6004(2) 0.61108(18) 0.0345(6) Uani 1 1 d . . . . .
O4 O -0.6199(4) 0.6076(2) 0.5013(2) 0.0397(6) Uani 1 1 d . . . . .
O5 O -0.9043(4) 0.5058(2) 0.89402(19) 0.0346(6) Uani 1 1 d . . . . .
O6 O -1.2445(4) 0.3812(2) 0.8851(2) 0.0438(7) Uani 1 1 d . . . . .
N1 N 0.1410(4) 1.3913(3) 0.9970(3) 0.0358(7) Uani 1 1 d . . . . .
N2 N 0.2291(4) 0.8776(3) 0.8823(3) 0.0397(8) Uani 1 1 d . . . . .
N3 N -0.6552(4) 0.4953(3) 0.6172(3) 0.0403(8) Uani 1 1 d . . . . .
C1 C 0.0802(6) 1.3137(3) 1.0104(4) 0.0439(9) Uani 1 1 d . . . . .
H1 H -0.0321 1.3078 1.0260 0.053 Uiso 1 1 calc R . . . .
C2 C 0.1738(6) 1.2401(4) 1.0026(4) 0.0454(10) Uani 1 1 d . . . . .
H2 H 0.1252 1.1852 1.0126 0.054 Uiso 1 1 calc R . . . .
C3 C 0.3387(5) 1.2472(3) 0.9800(3) 0.0349(8) Uani 1 1 d . . . . .
C4 C 0.4039(5) 1.3304(3) 0.9685(3) 0.0386(8) Uani 1 1 d . . . . .
H4 H 0.5171 1.3392 0.9544 0.046 Uiso 1 1 calc R . . . .
C5 C 0.3029(5) 1.4003(3) 0.9778(3) 0.0381(8) Uani 1 1 d . . . . .
H5 H 0.3497 1.4572 0.9704 0.046 Uiso 1 1 calc R . . . .
C6 C 0.4345(5) 1.1651(3) 0.9658(3) 0.0352(8) Uani 1 1 d . . . . .
C7 C 0.5564(7) 1.1522(4) 0.9075(4) 0.0488(11) Uani 1 1 d . . . . .
H7 H 0.5919 1.2043 0.8912 0.059 Uiso 1 1 calc R . . . .
C8 C 0.6301(6) 1.0673(3) 0.8713(3) 0.0425(9) Uani 1 1 d . . . . .
C9 C 0.7389(9) 1.0602(5) 0.7984(5) 0.0667(16) Uani 1 1 d . . . . .
H9A H 0.8477 1.0392 0.8153 0.100 Uiso 1 1 calc GR . . . .
H9B H 0.7740 1.1270 0.8024 0.100 Uiso 1 1 calc GR . . . .
H9C H 0.6658 1.0098 0.7300 0.100 Uiso 1 1 calc GR . . . .
C10 C 0.0787(5) 0.9082(3) 0.8912(3) 0.0409(9) Uani 1 1 d . . . . .
H10 H 0.0887 0.9733 0.9458 0.049 Uiso 1 1 calc R . . . .
C11 C -0.0901(5) 0.8521(3) 0.8270(3) 0.0388(8) Uani 1 1 d . . . . .
H11 H -0.1928 0.8781 0.8378 0.047 Uiso 1 1 calc R . . . .
C12 C -0.1091(5) 0.7566(3) 0.7457(3) 0.0343(8) Uani 1 1 d . . . . .
C13 C 0.0488(6) 0.7239(3) 0.7374(3) 0.0496(11) Uani 1 1 d . . . . .
H13 H 0.0436 0.6588 0.6842 0.059 Uiso 1 1 calc R . . . .
C14 C 0.2119(6) 0.7859(4) 0.8061(4) 0.0518(12) Uani 1 1 d . . . . .
H14 H 0.3173 0.7619 0.7987 0.062 Uiso 1 1 calc R . . . .
C15 C -0.2840(5) 0.6934(3) 0.6661(3) 0.0352(8) Uani 1 1 d . . . . .
C16 C -0.4193(6) 0.7413(3) 0.6558(4) 0.0512(11) Uani 1 1 d . . . . .
H16 H -0.4069 0.8078 0.7088 0.061 Uiso 1 1 calc R . . . .
C17 C -0.5730(5) 0.6989(3) 0.5730(3) 0.0447(9) Uani 1 1 d . . . . .
C18 C -0.6931(8) 0.7660(4) 0.5660(5) 0.0697(16) Uani 1 1 d . . . . .
H18A H -0.6966 0.7708 0.5047 0.104 Uiso 1 1 calc GR . . . .
H18B H -0.6454 0.8344 0.6248 0.104 Uiso 1 1 calc GR . . . .
H18C H -0.8157 0.7367 0.5640 0.104 Uiso 1 1 calc GR . . . .
C19 C -0.5849(6) 0.5149(4) 0.7099(3) 0.0512(11) Uani 1 1 d . . . . .
H19 H -0.4570 0.5359 0.7358 0.061 Uiso 1 1 calc R . . . .
C20 C -0.6887(6) 0.5066(4) 0.7725(3) 0.0526(12) Uani 1 1 d . . . . .
H20 H -0.6321 0.5190 0.8380 0.063 Uiso 1 1 calc R . . . .
C21 C -0.8753(5) 0.4798(3) 0.7365(3) 0.0351(8) Uani 1 1 d . . . . .
C22 C -0.9505(5) 0.4610(3) 0.6400(3) 0.0386(8) Uani 1 1 d . . . . .
H22 H -1.0780 0.4420 0.6126 0.046 Uiso 1 1 calc R . . . .
C23 C -0.8362(5) 0.4704(4) 0.5840(3) 0.0414(9) Uani 1 1 d . . . . .
H23 H -0.8890 0.4586 0.5182 0.050 Uiso 1 1 calc R . . . .
C24 C -0.9879(5) 0.4641(3) 0.8006(3) 0.0352(8) Uani 1 1 d . . . . .
C25 C -1.1636(6) 0.4037(4) 0.7536(3) 0.0520(12) Uani 1 1 d . . . . .
H25 H -1.2119 0.3873 0.6857 0.062 Uiso 1 1 calc R . . . .
C26 C -1.2804(6) 0.3634(4) 0.7962(3) 0.0461(10) Uani 1 1 d . . . . .
C27 C -1.4572(8) 0.2904(5) 0.7269(4) 0.0754(18) Uani 1 1 d . . . . .
H27A H -1.4433 0.2206 0.6979 0.113 Uiso 1 1 calc GR . . . .
H27B H -1.4967 0.3063 0.6729 0.113 Uiso 1 1 calc GR . . . .
H27C H -1.5477 0.2966 0.7644 0.113 Uiso 1 1 calc GR . . . .
O7 O -0.0556(15) 1.0179(8) 0.6178(8) 0.088(3) Uani 0.5 1 d . U . . .
C28 C -0.002(2) 0.9310(12) 0.6114(13) 0.088(4) Uani 0.5 1 d . U . . .
H28A H 0.0167 0.9325 0.6770 0.105 Uiso 0.5 1 calc R . . . .
H28B H 0.1134 0.9291 0.5927 0.105 Uiso 0.5 1 calc R . . . .
C30 C 0.0930(19) 1.1054(11) 0.6847(11) 0.080(3) Uani 0.5 1 d . U . . .
H30A H 0.1317 1.1077 0.7503 0.096 Uiso 0.5 1 calc R . . . .
H30B H 0.1970 1.1027 0.6558 0.096 Uiso 0.5 1 calc R . . . .
C29 C -0.148(2) 0.8394(13) 0.5331(14) 0.100(4) Uani 0.5 1 d . U . . .
H29A H -0.1370 0.8248 0.4662 0.150 Uiso 0.5 1 calc GR . . . .
H29B H -0.2662 0.8527 0.5389 0.150 Uiso 0.5 1 calc GR . . . .
H29C H -0.1374 0.7806 0.5426 0.150 Uiso 0.5 1 calc GR . . . .
C31 C 0.034(2) 1.1881(12) 0.6963(14) 0.098(5) Uani 0.5 1 d . U . . .
H31A H -0.0001 1.1859 0.6312 0.148 Uiso 0.5 1 calc GR . . . .
H31B H 0.1308 1.2500 0.7434 0.148 Uiso 0.5 1 calc GR . . . .
H31C H -0.0711 1.1886 0.7228 0.148 Uiso 0.5 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.963(3) . ?
Cu1 O1 1.963(3) 2_677 ?
Cu1 O2 1.989(3) 2_677 ?
Cu1 O2 1.989(3) . ?
Cu1 N2 2.376(3) 2_677 ?
Cu1 N2 2.376(3) . ?
Cu2 O3 1.966(3) . ?
Cu2 O3 1.966(3) 2_466 ?
Cu2 O4 1.988(3) 2_466 ?
Cu2 O4 1.988(3) . ?
Cu2 N3 2.375(3) . ?
Cu2 N3 2.375(3) 2_466 ?
Cu3 O5 1.952(2) 2_367 ?
Cu3 O5 1.952(2) . ?
Cu3 O6 2.221(3) 2_367 ?
Cu3 O6 2.221(3) . ?
Cu3 N1 2.097(3) 1_445 ?
Cu3 N1 2.097(3) 2_477 ?
O1 C6 1.274(5) . ?
O2 C8 1.251(5) . ?
O3 C15 1.268(5) . ?
O4 C17 1.270(5) . ?
O5 C24 1.279(5) . ?
O6 C26 1.246(5) . ?
N1 Cu3 2.097(3) 1_665 ?
N1 C1 1.320(5) . ?
N1 C5 1.347(5) . ?
N2 C10 1.328(5) . ?
N2 C14 1.327(5) . ?
N3 C19 1.317(6) . ?
N3 C23 1.341(5) . ?
C1 H1 0.9500 . ?
C1 C2 1.393(6) . ?
C2 H2 0.9500 . ?
C2 C3 1.391(5) . ?
C3 C4 1.388(6) . ?
C3 C6 1.496(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.381(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.400(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.409(6) . ?
C8 C9 1.504(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 0.9500 . ?
C10 C11 1.372(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.393(5) . ?
C12 C13 1.396(5) . ?
C12 C15 1.498(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.376(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.389(6) . ?
C16 H16 0.9500 . ?
C16 C17 1.404(6) . ?
C17 C18 1.504(6) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19 0.9500 . ?
C19 C20 1.404(5) . ?
C20 H20 0.9500 . ?
C20 C21 1.384(6) . ?
C21 C22 1.383(5) . ?
C21 C24 1.509(5) . ?
C22 H22 0.9500 . ?
C22 C23 1.384(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.383(6) . ?
C25 H25 0.9500 . ?
C25 C26 1.433(5) . ?
C26 C27 1.492(7) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
O7 C28 1.409(16) . ?
O7 C30 1.434(17) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.49(2) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.34(2) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O1 180.0 . 2_677 ?
O1 Cu1 O2 87.18(11) 2_677 . ?
O1 Cu1 O2 92.82(11) . . ?
O1 Cu1 O2 92.82(11) 2_677 2_677 ?
O1 Cu1 O2 87.18(11) . 2_677 ?
O1 Cu1 N2 90.04(12) . 2_677 ?
O1 Cu1 N2 90.04(12) 2_677 . ?
O1 Cu1 N2 89.96(12) 2_677 2_677 ?
O1 Cu1 N2 89.96(12) . . ?
O2 Cu1 O2 180.0 2_677 . ?
O2 Cu1 N2 93.21(12) 2_677 2_677 ?
O2 Cu1 N2 86.79(12) 2_677 . ?
O2 Cu1 N2 93.21(12) . . ?
O2 Cu1 N2 86.79(12) . 2_677 ?
N2 Cu1 N2 180.0 2_677 . ?
O3 Cu2 O3 180.00(12) . 2_466 ?
O3 Cu2 O4 87.35(11) 2_466 . ?
O3 Cu2 O4 92.64(11) . . ?
O3 Cu2 O4 87.36(11) . 2_466 ?
O3 Cu2 O4 92.65(11) 2_466 2_466 ?
O3 Cu2 N3 89.78(11) 2_466 . ?
O3 Cu2 N3 90.22(11) . . ?
O3 Cu2 N3 89.78(11) . 2_466 ?
O3 Cu2 N3 90.22(11) 2_466 2_466 ?
O4 Cu2 O4 180.0 2_466 . ?
O4 Cu2 N3 86.23(12) . . ?
O4 Cu2 N3 93.77(12) 2_466 . ?
O4 Cu2 N3 93.76(12) . 2_466 ?
O4 Cu2 N3 86.23(12) 2_466 2_466 ?
N3 Cu2 N3 180.0 . 2_466 ?
O5 Cu3 O5 180.00(6) 2_367 . ?
O5 Cu3 O6 90.13(11) . . ?
O5 Cu3 O6 89.87(11) 2_367 . ?
O5 Cu3 O6 90.13(11) 2_367 2_367 ?
O5 Cu3 O6 89.87(11) . 2_367 ?
O5 Cu3 N1 89.53(12) . 1_445 ?
O5 Cu3 N1 89.53(12) 2_367 2_477 ?
O5 Cu3 N1 90.47(12) . 2_477 ?
O5 Cu3 N1 90.47(12) 2_367 1_445 ?
O6 Cu3 O6 180.0 2_367 . ?
N1 Cu3 O6 87.29(13) 1_445 2_367 ?
N1 Cu3 O6 92.71(13) 2_477 2_367 ?
N1 Cu3 O6 92.70(13) 1_445 . ?
N1 Cu3 O6 87.30(13) 2_477 . ?
N1 Cu3 N1 180.0(2) 2_477 1_445 ?
C6 O1 Cu1 123.9(2) . . ?
C8 O2 Cu1 123.8(2) . . ?
C15 O3 Cu2 124.3(3) . . ?
C17 O4 Cu2 123.8(3) . . ?
C24 O5 Cu3 127.1(2) . . ?
C26 O6 Cu3 121.1(3) . . ?
C1 N1 Cu3 124.5(3) . 1_665 ?
C1 N1 C5 117.9(3) . . ?
C5 N1 Cu3 117.6(3) . 1_665 ?
C10 N2 Cu1 115.1(3) . . ?
C14 N2 Cu1 127.9(3) . . ?
C14 N2 C10 116.8(4) . . ?
C19 N3 Cu2 127.9(3) . . ?
C19 N3 C23 117.0(3) . . ?
C23 N3 Cu2 115.1(3) . . ?
N1 C1 H1 118.6 . . ?
N1 C1 C2 122.7(4) . . ?
C2 C1 H1 118.6 . . ?
C1 C2 H2 120.1 . . ?
C3 C2 C1 119.7(4) . . ?
C3 C2 H2 120.1 . . ?
C2 C3 C6 119.8(4) . . ?
C4 C3 C2 117.2(4) . . ?
C4 C3 C6 122.9(3) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 C3 119.4(3) . . ?
C5 C4 H4 120.3 . . ?
N1 C5 C4 123.0(4) . . ?
N1 C5 H5 118.5 . . ?
C4 C5 H5 118.5 . . ?
O1 C6 C3 116.0(3) . . ?
O1 C6 C7 126.1(4) . . ?
C7 C6 C3 117.9(4) . . ?
C6 C7 H7 117.8 . . ?
C6 C7 C8 124.5(4) . . ?
C8 C7 H7 117.8 . . ?
O2 C8 C7 126.0(4) . . ?
O2 C8 C9 117.3(4) . . ?
C7 C8 C9 116.6(4) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 H10 117.8 . . ?
N2 C10 C11 124.5(4) . . ?
C11 C10 H10 117.8 . . ?
C10 C11 H11 120.4 . . ?
C10 C11 C12 119.1(4) . . ?
C12 C11 H11 120.4 . . ?
C11 C12 C13 116.3(4) . . ?
C11 C12 C15 123.4(3) . . ?
C13 C12 C15 120.2(3) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 C12 120.0(4) . . ?
C14 C13 H13 120.0 . . ?
N2 C14 C13 123.2(4) . . ?
N2 C14 H14 118.4 . . ?
C13 C14 H14 118.4 . . ?
O3 C15 C12 115.3(3) . . ?
O3 C15 C16 126.2(4) . . ?
C16 C15 C12 118.4(4) . . ?
C15 C16 H16 117.5 . . ?
C15 C16 C17 125.0(4) . . ?
C17 C16 H16 117.5 . . ?
O4 C17 C16 125.5(4) . . ?
O4 C17 C18 116.0(4) . . ?
C16 C17 C18 118.5(4) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 H19 118.2 . . ?
N3 C19 C20 123.7(4) . . ?
C20 C19 H19 118.2 . . ?
C19 C20 H20 120.8 . . ?
C21 C20 C19 118.4(4) . . ?
C21 C20 H20 120.8 . . ?
C20 C21 C24 118.8(3) . . ?
C22 C21 C20 118.4(3) . . ?
C22 C21 C24 122.7(3) . . ?
C21 C22 H22 120.7 . . ?
C21 C22 C23 118.7(4) . . ?
C23 C22 H22 120.7 . . ?
N3 C23 C22 123.8(4) . . ?
N3 C23 H23 118.1 . . ?
C22 C23 H23 118.1 . . ?
O5 C24 C21 114.7(3) . . ?
O5 C24 C25 127.1(3) . . ?
C25 C24 C21 118.1(3) . . ?
C24 C25 H25 116.6 . . ?
C24 C25 C26 126.9(4) . . ?
C26 C25 H25 116.6 . . ?
O6 C26 C25 125.7(4) . . ?
O6 C26 C27 117.3(4) . . ?
C25 C26 C27 116.9(4) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C28 O7 C30 107.6(12) . . ?
O7 C28 H28A 110.2 . . ?
O7 C28 H28B 110.2 . . ?
O7 C28 C29 107.4(13) . . ?
H28A C28 H28B 108.5 . . ?
C29 C28 H28A 110.2 . . ?
C29 C28 H28B 110.2 . . ?
O7 C30 H30A 110.4 . . ?
O7 C30 H30B 110.4 . . ?
H30A C30 H30B 108.6 . . ?
C31 C30 O7 106.7(13) . . ?
C31 C30 H30A 110.4 . . ?
C31 C30 H30B 110.4 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 O1 C6 C3 -178.7(2) . . . . ?
Cu1 O1 C6 C7 4.1(6) . . . . ?
Cu1 O2 C8 C7 -8.7(7) . . . . ?
Cu1 O2 C8 C9 172.1(4) . . . . ?
Cu1 N2 C10 C11 175.5(4) . . . . ?
Cu1 N2 C14 C13 -174.7(4) . . . . ?
Cu2 O3 C15 C12 -179.3(2) . . . . ?
Cu2 O3 C15 C16 -2.8(6) . . . . ?
Cu2 O4 C17 C16 7.8(7) . . . . ?
Cu2 O4 C17 C18 -173.1(4) . . . . ?
Cu2 N3 C19 C20 -177.7(4) . . . . ?
Cu2 N3 C23 C22 178.2(4) . . . . ?
Cu3 O5 C24 C21 -178.2(2) . . . . ?
Cu3 O5 C24 C25 -1.4(6) . . . . ?
Cu3 O6 C26 C25 9.2(7) . . . . ?
Cu3 O6 C26 C27 -173.6(4) . . . . ?
Cu3 N1 C1 C2 176.5(4) 1_665 . . . ?
Cu3 N1 C5 C4 -176.4(3) 1_665 . . . ?
O1 C6 C7 C8 9.9(8) . . . . ?
O3 C15 C16 C17 -10.8(8) . . . . ?
O5 C24 C25 C26 -9.6(8) . . . . ?
N1 C1 C2 C3 0.2(8) . . . . ?
N2 C10 C11 C12 -0.5(7) . . . . ?
N3 C19 C20 C21 -2.4(9) . . . . ?
C1 N1 C5 C4 2.1(7) . . . . ?
C1 C2 C3 C4 1.4(7) . . . . ?
C1 C2 C3 C6 -176.6(4) . . . . ?
C2 C3 C4 C5 -1.2(6) . . . . ?
C2 C3 C6 O1 -21.5(6) . . . . ?
C2 C3 C6 C7 155.9(5) . . . . ?
C3 C4 C5 N1 -0.5(7) . . . . ?
C3 C6 C7 C8 -167.2(4) . . . . ?
C4 C3 C6 O1 160.6(4) . . . . ?
C4 C3 C6 C7 -22.0(6) . . . . ?
C5 N1 C1 C2 -1.9(7) . . . . ?
C6 C3 C4 C5 176.7(4) . . . . ?
C6 C7 C8 O2 -7.2(8) . . . . ?
C6 C7 C8 C9 172.0(5) . . . . ?
C10 N2 C14 C13 0.9(8) . . . . ?
C10 C11 C12 C13 1.4(7) . . . . ?
C10 C11 C12 C15 -174.4(4) . . . . ?
C11 C12 C13 C14 -1.3(8) . . . . ?
C11 C12 C15 O3 -164.6(4) . . . . ?
C11 C12 C15 C16 18.6(6) . . . . ?
C12 C13 C14 N2 0.1(9) . . . . ?
C12 C15 C16 C17 165.6(5) . . . . ?
C13 C12 C15 O3 19.7(6) . . . . ?
C13 C12 C15 C16 -157.1(5) . . . . ?
C14 N2 C10 C11 -0.7(7) . . . . ?
C15 C12 C13 C14 174.7(5) . . . . ?
C15 C16 C17 O4 7.9(9) . . . . ?
C15 C16 C17 C18 -171.2(5) . . . . ?
C19 N3 C23 C22 -2.4(7) . . . . ?
C19 C20 C21 C22 1.0(8) . . . . ?
C19 C20 C21 C24 176.1(4) . . . . ?
C20 C21 C22 C23 -0.5(7) . . . . ?
C20 C21 C24 O5 20.1(6) . . . . ?
C20 C21 C24 C25 -157.0(5) . . . . ?
C21 C22 C23 N3 1.2(7) . . . . ?
C21 C24 C25 C26 167.2(5) . . . . ?
C22 C21 C24 O5 -165.0(4) . . . . ?
C22 C21 C24 C25 17.9(6) . . . . ?
C23 N3 C19 C20 3.0(8) . . . . ?
C24 C21 C22 C23 -175.4(4) . . . . ?
C24 C25 C26 O6 4.1(9) . . . . ?
C24 C25 C26 C27 -173.2(5) . . . . ?
C28 O7 C30 C31 -175.1(12) . . . . ?
C30 O7 C28 C29 -173.7(11) . . . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 -8 9 0.0100 0.0577 -7.9099 8.9297 -0.9712 -0.1809 0.1554
0 -5 1 0.0283 -0.0001 -4.9954 1.4978 -0.4121 0.3217 0.0588
0 -3 -7 0.0346 0.1708 -2.9172 -6.8875 0.1293 0.9879 -0.0858
5 0 -4 0.0869 4.9640 -0.2488 -3.5833 0.0048 0.0465 -0.9989
0 3 7 0.0098 0.3026 2.9172 6.6009 -0.1299 -0.9915 -0.0091
-5 -1 0 0.0917 -4.6631 -1.0727 0.3280 0.0535 0.3993 0.9153
-1 8 -9 0.0263 -0.5753 8.0070 -8.6850 0.9817 0.1827 -0.0533

_olex2_date_sample_data_collection 15/12/14
_olex2_date_sample_submission    15/12/14
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id PC1469
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_MeOH_156_Lab
_database_code_depnum_ccdc_archive 'CCDC 1564971'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2020-06-09 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_audit_creation_date             2017-05-19
_audit_creation_method           CRYSTALS_ver_14.61_build_6236

_oxford_structure_analysis_title 'ST6105_0m in R-3'
_chemical_name_systematic        ?
_chemical_melting_point          ?

#end of refcif 
_cell_length_a                   25.4345(8)
_cell_length_b                   25.4345(8)
_cell_length_c                   7.7363(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4334.2(3)

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3

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            9

# Given Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.34 Fooo =   1791.00 Mu =     11.56 M =    387.88
# Found Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.34 FOOO =   1791.00 Mu =     11.56 M =    387.88

_chemical_formula_sum            'C18 H16 Cu1 N2 O4'
_chemical_formula_moiety         'C18 H16 Cu1 N2 O4'
_chemical_compound_source        ?
_chemical_formula_weight         387.88


_cell_measurement_reflns_used    2414
_cell_measurement_theta_min      3
_cell_measurement_theta_max      24
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1791
_exptl_absorpt_coefficient_mu    1.156

# Sheldrick geometric approximatio 0.79 0.89 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_T_max  0.89
_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            4972
_reflns_number_total             1202
_diffrn_reflns_av_R_equivalents  0.041
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 1202 
# Theoretical number of reflections is about 3173 


_diffrn_reflns_theta_min         3.218
_diffrn_reflns_theta_max         24.411
_diffrn_measured_fraction_theta_max 0.760

_diffrn_reflns_theta_full        18.308
_diffrn_measured_fraction_theta_full 0.828


_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_reflns_limit_h_min              -26
_reflns_limit_h_max              12
_reflns_limit_k_min              0
_reflns_limit_k_max              29
_reflns_limit_l_min              0
_reflns_limit_l_max              8

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.40
_refine_diff_density_max         0.45


# 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         1199
_refine_ls_number_restraints     126
_refine_ls_number_parameters     115
_oxford_refine_ls_R_factor_ref   0.0574
_refine_ls_wR_factor_ref         0.1047
_refine_ls_goodness_of_fit_ref   0.9951
_refine_ls_shift/su_max          0.0001433
_refine_ls_shift/su_mean         0.0000170


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1199
_refine_ls_R_factor_all          0.0574
_refine_ls_wR_factor_all         0.1047

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                980
_refine_ls_R_factor_gt           0.0442
_refine_ls_wR_factor_gt          0.0978

# 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) + ( 0.03P)² +40.82P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# 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 0.8333 0.6667 0.6667 0.0324 1.0000 Uani S . . . . .
O2 O 0.75771(13) 0.63492(14) 0.5349(4) 0.0397 1.0000 Uani D U . . . .
C4 C 0.70581(17) 0.59160(18) 0.5822(5) 0.0349 1.0000 Uani D U . . . .
C5 C 0.65642(16) 0.57321(18) 0.4506(5) 0.0343 1.0000 Uani D U . . . .
C6 C 0.67110(19) 0.5973(2) 0.2850(5) 0.0494 1.0000 Uani D U . . . .
C7 C 0.62717(19) 0.5763(2) 0.1585(5) 0.0479 1.0000 Uani D U . . . .
N1 N 0.57013(16) 0.53372(16) 0.1859(4) 0.0388 1.0000 Uani D U . . . .
C9 C 0.55596(19) 0.5122(2) 0.3472(5) 0.0450 1.0000 Uani D U . . . .
C8 C 0.59661(18) 0.5306(2) 0.4810(5) 0.0395 1.0000 Uani D U . . . .
C3 C 0.6929(2) 0.5582(2) 0.7328(6) 0.0497 1.0000 Uani D U . . . .
C2 C 0.73590(19) 0.5547(2) 0.8408(5) 0.0475 1.0000 Uani D U . . . .
O1 O 0.79213(14) 0.58515(15) 0.8234(4) 0.0496 1.0000 Uani D U . . . .
C1 C 0.7121(3) 0.5077(3) 0.9819(7) 0.0806 1.0000 Uani D U . . . .
H61 H 0.7114 0.6282 0.2592 0.0596 1.0000 Uiso R . . . . .
H71 H 0.6384 0.5931 0.0458 0.0572 1.0000 Uiso R . . . . .
H91 H 0.5151 0.4821 0.3702 0.0542 1.0000 Uiso R . . . . .
H81 H 0.5836 0.5143 0.5935 0.0474 1.0000 Uiso R . . . . .
H31 H 0.6515 0.5357 0.7671 0.0603 1.0000 Uiso R . . . . .
H11 H 0.7402 0.4925 1.0003 0.0967 1.0000 Uiso R . . . . .
H12 H 0.7082 0.5257 1.0894 0.0967 1.0000 Uiso R . . . . .
H13 H 0.6724 0.4741 0.9495 0.0967 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.07259(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 6_666 2.167(3) yes
Cu1 . N1 9_655 2.111(3) yes
Cu1 . N1 10_555 2.111(3) yes
Cu1 . O2 6_666 1.959(3) yes
Cu1 . O2 . 1.959(3) yes
Cu1 . O1 . 2.167(3) yes
O2 . C4 . 1.279(4) yes
C4 . C5 . 1.499(5) yes
C4 . C3 . 1.381(5) yes
C5 . C6 . 1.388(5) yes
C5 . C8 . 1.376(5) yes
C6 . C7 . 1.377(5) yes
C6 . H61 . 0.950 no
C7 . N1 . 1.323(5) yes
C7 . H71 . 0.950 no
N1 . C9 . 1.337(5) yes
C9 . C8 . 1.370(5) yes
C9 . H91 . 0.950 no
C8 . H81 . 0.950 no
C3 . C2 . 1.414(5) yes
C3 . H31 . 0.950 no
C2 . O1 . 1.247(4) yes
C2 . C1 . 1.505(5) yes
C1 . H11 . 0.979 no
C1 . H12 . 0.977 no
C1 . H13 . 0.974 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 6_666 Cu1 . N1 9_655 94.00(13) yes
O1 6_666 Cu1 . N1 10_555 86.00(13) yes
N1 9_655 Cu1 . N1 10_555 179.995 yes
O1 6_666 Cu1 . O2 6_666 89.50(12) yes
N1 9_655 Cu1 . O2 6_666 89.73(12) yes
N1 10_555 Cu1 . O2 6_666 90.27(12) yes
O1 6_666 Cu1 . O2 . 90.50(12) yes
N1 9_655 Cu1 . O2 . 90.27(12) yes
N1 10_555 Cu1 . O2 . 89.73(12) yes
O2 6_666 Cu1 . O2 . 179.994 yes
O1 6_666 Cu1 . O1 . 179.995 yes
N1 9_655 Cu1 . O1 . 86.00(13) yes
N1 10_555 Cu1 . O1 . 94.00(13) yes
O2 6_666 Cu1 . O1 . 90.50(12) yes
O2 . Cu1 . O1 . 89.50(12) yes
Cu1 . O2 . C4 . 125.7(2) yes
O2 . C4 . C5 . 114.7(3) yes
O2 . C4 . C3 . 126.7(3) yes
C5 . C4 . C3 . 118.4(3) yes
C4 . C5 . C6 . 119.4(3) yes
C4 . C5 . C8 . 123.6(3) yes
C6 . C5 . C8 . 116.9(3) yes
C5 . C6 . C7 . 119.9(4) yes
C5 . C6 . H61 . 120.0 no
C7 . C6 . H61 . 120.1 no
C6 . C7 . N1 . 123.2(4) yes
C6 . C7 . H71 . 118.3 no
N1 . C7 . H71 . 118.4 no
C7 . N1 . Cu1 16_545 125.5(3) yes
C7 . N1 . C9 . 116.4(3) yes
Cu1 16_545 N1 . C9 . 118.0(3) yes
N1 . C9 . C8 . 124.2(4) yes
N1 . C9 . H91 . 117.8 no
C8 . C9 . H91 . 118.0 no
C5 . C8 . C9 . 119.2(3) yes
C5 . C8 . H81 . 120.5 no
C9 . C8 . H81 . 120.3 no
C4 . C3 . C2 . 125.6(4) yes
C4 . C3 . H31 . 117.2 no
C2 . C3 . H31 . 117.2 no
C3 . C2 . O1 . 125.5(4) yes
C3 . C2 . C1 . 117.5(4) yes
O1 . C2 . C1 . 116.9(4) yes
Cu1 . O1 . C2 . 120.7(3) yes
C2 . C1 . H11 . 109.6 no
C2 . C1 . H12 . 109.9 no
H11 . C1 . H12 . 109.0 no
C2 . C1 . H13 . 109.8 no
H11 . C1 . H13 . 109.3 no
H12 . C1 . H13 . 109.1 no


# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 
# looking for PLATON_SQD.SQF 

# SQUEEZE RESULTS (Version =  60516) 
# Note: Data are Listed for all Voids in the P1 Unit Cell 
# i.e. Centre of Gravity, Solvent Accessible Volume, 
# Recovered number of Electrons in the Void and 
# Details about the Squeezed Material 
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 -0.013 344 112 ' '
2 0.333 0.667 -0.179 347 113 ' '
3 0.667 0.333 0.095 347 113 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_MeOH_128_Lab
_database_code_depnum_ccdc_archive 'CCDC 1564970'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2020-06-09 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_audit_creation_date             2017-05-19
_audit_creation_method           CRYSTALS_ver_14.61_build_6236

_oxford_structure_analysis_title 'ST6100_0m in R-3'
_chemical_name_systematic        ?
_chemical_melting_point          ?

#end of refcif 
_cell_length_a                   25.6002(12)
_cell_length_b                   25.6002(12)
_cell_length_c                   7.7386(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4392.2(4)

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3

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            9

# Given Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.32 Fooo =   1791.00 Mu =     11.41 M =    387.88
# Found Formula = C18 H16 Cu1 N2 O4 
# Dc =      1.32 FOOO =   1791.00 Mu =     11.41 M =    387.88

_chemical_formula_sum            'C18 H16 Cu1 N2 O4'
_chemical_formula_moiety         'C18 H16 Cu1 N2 O4'
_chemical_compound_source        ?
_chemical_formula_weight         387.88


_cell_measurement_reflns_used    2610
_cell_measurement_theta_min      3
_cell_measurement_theta_max      24
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1791
_exptl_absorpt_coefficient_mu    1.141

# Sheldrick geometric approximatio 0.80 0.89 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_T_max  0.89
_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            4864
_reflns_number_total             1188
_diffrn_reflns_av_R_equivalents  0.038
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 1188 
# Theoretical number of reflections is about 3212 


_diffrn_reflns_theta_min         3.210
_diffrn_reflns_theta_max         24.401
_diffrn_measured_fraction_theta_max 0.739

_diffrn_reflns_theta_full        18.301
_diffrn_measured_fraction_theta_full 0.835


_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_reflns_limit_h_min              -26
_reflns_limit_h_max              13
_reflns_limit_k_min              0
_reflns_limit_k_max              29
_reflns_limit_l_min              0
_reflns_limit_l_max              8

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.75
_refine_diff_density_max         0.75


# 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         1185
_refine_ls_number_restraints     126
_refine_ls_number_parameters     115
_oxford_refine_ls_R_factor_ref   0.0766
_refine_ls_wR_factor_ref         0.2222
_refine_ls_goodness_of_fit_ref   1.1201
_refine_ls_shift/su_max          0.0001195
_refine_ls_shift/su_mean         0.0000165


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1185
_refine_ls_R_factor_all          0.0766
_refine_ls_wR_factor_all         0.2222

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                964
_refine_ls_R_factor_gt           0.0622
_refine_ls_wR_factor_gt          0.2005

# 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) + ( 0.11P)² +73.94P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# 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 0.8333 0.6667 0.6667 0.0337 1.0000 Uani S . . . . .
O2 O 0.7582(2) 0.6342(2) 0.5342(6) 0.0440 1.0000 Uani D U . . . .
C4 C 0.7066(2) 0.5918(3) 0.5815(7) 0.0386 1.0000 Uani D U . . . .
C5 C 0.6577(2) 0.5738(3) 0.4503(7) 0.0359 1.0000 Uani D U . . . .
C6 C 0.6716(3) 0.5964(4) 0.2842(9) 0.0534 1.0000 Uani D U . . . .
C7 C 0.6280(3) 0.5764(4) 0.1584(9) 0.0530 1.0000 Uani D U . . . .
N1 N 0.5711(3) 0.5352(3) 0.1872(7) 0.0468 1.0000 Uani D U . . . .
C9 C 0.5575(3) 0.5140(3) 0.3494(8) 0.0494 1.0000 Uani D U . . . .
C8 C 0.5982(3) 0.5326(3) 0.4828(8) 0.0436 1.0000 Uani D U . . . .
C3 C 0.6944(3) 0.5592(4) 0.7330(9) 0.0521 1.0000 Uani D U . . . .
C2 C 0.7375(3) 0.5548(3) 0.8375(9) 0.0511 1.0000 Uani D U . . . .
O1 O 0.7936(2) 0.5870(3) 0.8219(7) 0.0541 1.0000 Uani D U . . . .
C1 C 0.7153(4) 0.5094(5) 0.9798(12) 0.0803 1.0000 Uani D U . . . .
H61 H 0.7115 0.6262 0.2543 0.0620 1.0000 Uiso R . . . . .
H71 H 0.6391 0.5930 0.0456 0.0607 1.0000 Uiso R . . . . .
H91 H 0.5169 0.4844 0.3739 0.0626 1.0000 Uiso R . . . . .
H81 H 0.5856 0.5170 0.5960 0.0510 1.0000 Uiso R . . . . .
H31 H 0.6536 0.5376 0.7696 0.0708 1.0000 Uiso R . . . . .
H11 H 0.7495 0.5098 1.0384 0.0932 1.0000 Uiso R . . . . .
H12 H 0.6930 0.5198 1.0624 0.0932 1.0000 Uiso R . . . . .
H13 H 0.6885 0.4690 0.9330 0.0932 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.07019(7)
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 . N1 9_655 2.141(5) yes
Cu1 . N1 10_555 2.141(5) yes
Cu1 . O1 6_666 2.136(6) yes
Cu1 . O2 6_666 1.961(5) yes
Cu1 . O2 . 1.961(5) yes
Cu1 . O1 . 2.136(6) yes
O2 . C4 . 1.274(6) yes
C4 . C5 . 1.496(6) yes
C4 . C3 . 1.380(7) yes
C5 . C6 . 1.381(7) yes
C5 . C8 . 1.374(7) yes
C6 . C7 . 1.372(7) yes
C6 . H61 . 0.950 no
C7 . N1 . 1.322(7) yes
C7 . H71 . 0.950 no
N1 . C9 . 1.342(7) yes
C9 . C8 . 1.372(7) yes
C9 . H91 . 0.950 no
C8 . H81 . 0.950 no
C3 . C2 . 1.416(7) yes
C3 . H31 . 0.950 no
C2 . O1 . 1.253(6) yes
C2 . C1 . 1.493(7) yes
C1 . H11 . 0.980 no
C1 . H12 . 0.980 no
C1 . H13 . 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
N1 9_655 Cu1 . N1 10_555 179.995 yes
N1 9_655 Cu1 . O1 6_666 94.2(2) yes
N1 10_555 Cu1 . O1 6_666 85.8(2) yes
N1 9_655 Cu1 . O2 6_666 89.9(2) yes
N1 10_555 Cu1 . O2 6_666 90.1(2) yes
O1 6_666 Cu1 . O2 6_666 89.5(2) yes
N1 9_655 Cu1 . O2 . 90.1(2) yes
N1 10_555 Cu1 . O2 . 89.9(2) yes
O1 6_666 Cu1 . O2 . 90.5(2) yes
O2 6_666 Cu1 . O2 . 179.994 yes
N1 9_655 Cu1 . O1 . 85.8(2) yes
N1 10_555 Cu1 . O1 . 94.2(2) yes
O1 6_666 Cu1 . O1 . 179.995 yes
O2 6_666 Cu1 . O1 . 90.5(2) yes
O2 . Cu1 . O1 . 89.5(2) yes
Cu1 . O2 . C4 . 126.1(4) yes
O2 . C4 . C5 . 114.7(4) yes
O2 . C4 . C3 . 125.8(5) yes
C5 . C4 . C3 . 119.3(4) yes
C4 . C5 . C6 . 120.2(4) yes
C4 . C5 . C8 . 123.2(4) yes
C6 . C5 . C8 . 116.5(4) yes
C5 . C6 . C7 . 120.9(5) yes
C5 . C6 . H61 . 120.7 no
C7 . C6 . H61 . 118.4 no
C6 . C7 . N1 . 123.0(5) yes
C6 . C7 . H71 . 118.6 no
N1 . C7 . H71 . 118.4 no
C7 . N1 . Cu1 16_545 126.0(4) yes
C7 . N1 . C9 . 116.1(5) yes
Cu1 16_545 N1 . C9 . 118.0(4) yes
N1 . C9 . C8 . 124.4(5) yes
N1 . C9 . H91 . 117.9 no
C8 . C9 . H91 . 117.7 no
C5 . C8 . C9 . 119.1(5) yes
C5 . C8 . H81 . 120.4 no
C9 . C8 . H81 . 120.5 no
C4 . C3 . C2 . 125.6(5) yes
C4 . C3 . H31 . 117.1 no
C2 . C3 . H31 . 117.2 no
C3 . C2 . O1 . 125.0(5) yes
C3 . C2 . C1 . 118.4(5) yes
O1 . C2 . C1 . 116.6(5) yes
Cu1 . O1 . C2 . 121.6(4) yes
C2 . C1 . H11 . 110.1 no
C2 . C1 . H12 . 108.3 no
H11 . C1 . H12 . 109.5 no
C2 . C1 . H13 . 110.0 no
H11 . C1 . H13 . 109.5 no
H12 . C1 . H13 . 109.4 no


# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 
# looking for PLATON_SQD.SQF 

# SQUEEZE RESULTS (Version =  60516) 
# Note: Data are Listed for all Voids in the P1 Unit Cell 
# i.e. Centre of Gravity, Solvent Accessible Volume, 
# Recovered number of Electrons in the Void and 
# Details about the Squeezed Material 
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 -0.012 357 134 ' '
2 0.333 0.667 -0.179 360 134 ' '
3 0.667 0.333 0.086 360 134 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?
