# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Parthasarathi Dastidar'
_publ_contact_author_address     
;
ORGANIC CHEMISTRY
INDIAN ASSOCIATION FOR THE CULTIVATION OF SCIENCE
2A AND 2B RAJA S C MULLICK ROAD, JA
KOLKATA
WEST BENGAL
700032
INDIA
;

_publ_contact_author_email       PARTHOD123@REDIFFMAIL.COM

_publ_section_title              
;
An unprecedented all helical 3D network and a rarely
observed non-interpenetrated octahedral network in homochiral Cu(II)
MOFs: Effect of steric bulk and ?-? stacking interactions of the
ligand backbone
;
loop_
_publ_author_name
'Parthasarathi Dastidar'
N.N.Adrash
'Subhabrata Banerjee'
# Attachment 'MOF 1 ANN129A1_FINAL_R1.cif'

data_test
_database_code_depnum_ccdc_archive 'CCDC 699625'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_absolute_configuration syn
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H40 Cl2 Cu N8 O6'
_chemical_formula_weight         863.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           TRIGONAL
_symmetry_space_group_name_H-M   P3(2)21

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'y, x, -z'
'x-y, -y, -z+1/3'
'-x, -x+y, -z+2/3'

_cell_length_a                   12.9207(3)
_cell_length_b                   12.9207(3)
_cell_length_c                   19.9320(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2881.73(17)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            BLUE
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1341
_exptl_absorpt_coefficient_mu    0.768
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.7591
_exptl_absorpt_correction_T_max  0.9135
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER CCD AREA DETECTOR'
_diffrn_measurement_method       'PHI-OMEGA SCAN'
_diffrn_detector_area_resol_mean 3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34199
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.82
_diffrn_reflns_theta_max         32.02
_reflns_number_total             6026
_reflns_number_gt                5364
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER AXS SMART 3'
_computing_cell_refinement       'BRUKER AXS SMART 3'
_computing_data_reduction        'BRUKER AXS SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'BRUKER SHELXLTL'
_computing_publication_material  'MERCURY 1.4'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0511P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.007(8)
_refine_ls_number_reflns         6026
_refine_ls_number_parameters     266
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0332
_refine_ls_wR_factor_ref         0.0817
_refine_ls_wR_factor_gt          0.0787
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.62121(2) 0.0000 1.1667 0.01507(7) Uani 1 2 d S . .
Cl1 Cl 0.74236(4) 0.24402(4) 1.139727(19) 0.02142(9) Uani 1 1 d . . .
N1 N 0.49621(12) -0.02299(12) 1.09642(6) 0.0154(3) Uani 1 1 d . . .
C2 C 0.52791(14) 0.03898(14) 1.03853(7) 0.0164(3) Uani 1 1 d . . .
H2 H 0.6069 0.0989 1.0328 0.020 Uiso 1 1 calc R . .
C3 C 0.44710(15) 0.01675(14) 0.98713(7) 0.0167(3) Uani 1 1 d . . .
C4 C 0.32806(16) -0.07048(15) 0.99715(8) 0.0207(3) Uani 1 1 d . . .
H4 H 0.2718 -0.0873 0.9636 0.025 Uiso 1 1 calc R . .
C5 C 0.29451(15) -0.13157(16) 1.05710(8) 0.0213(3) Uani 1 1 d . . .
H5 H 0.2150 -0.1881 1.0652 0.026 Uiso 1 1 calc R . .
C6 C 0.38126(15) -0.10741(15) 1.10515(8) 0.0185(3) Uani 1 1 d . . .
H6 H 0.3591 -0.1512 1.1448 0.022 Uiso 1 1 calc R . .
C7 C 0.49279(14) 0.08801(14) 0.92383(8) 0.0179(3) Uani 1 1 d . . .
O8 O 0.57806(12) 0.19116(11) 0.92468(6) 0.0249(3) Uani 1 1 d . . .
N9 N 0.43408(14) 0.03095(13) 0.86797(7) 0.0211(3) Uani 1 1 d . . .
H9 H 0.3767 -0.0418 0.8711 0.025 Uiso 1 1 calc R . .
C10 C 0.46392(16) 0.08769(16) 0.80237(8) 0.0213(3) Uani 1 1 d . . .
H10 H 0.5280 0.1709 0.8070 0.026 Uiso 1 1 calc R . .
C11 C 0.50374(19) 0.02229(17) 0.75396(8) 0.0274(4) Uani 1 1 d . . .
H11A H 0.4430 -0.0617 0.7541 0.033 Uiso 1 1 calc R . .
H11B H 0.5056 0.0524 0.7091 0.033 Uiso 1 1 calc R . .
C12 C 0.62204(18) 0.03096(18) 0.76680(8) 0.0280(4) Uani 1 1 d . . .
C13 C 0.6323(2) -0.0710(2) 0.76369(12) 0.0438(6) Uani 1 1 d . . .
H13 H 0.5638 -0.1452 0.7585 0.053 Uiso 1 1 calc R . .
C14 C 0.7414(3) -0.0646(2) 0.76808(13) 0.0511(7) Uani 1 1 d . . .
H14 H 0.7458 -0.1341 0.7651 0.061 Uiso 1 1 calc R . .
C15 C 0.8446(2) 0.0439(3) 0.77694(11) 0.0449(6) Uani 1 1 d . . .
H15 H 0.9181 0.0479 0.7814 0.054 Uiso 1 1 calc R . .
C16 C 0.8364(2) 0.1465(2) 0.77904(12) 0.0445(6) Uani 1 1 d . . .
H16 H 0.9051 0.2205 0.7841 0.053 Uiso 1 1 calc R . .
C17 C 0.7262(2) 0.1396(2) 0.77364(11) 0.0382(5) Uani 1 1 d . . .
H17 H 0.7223 0.2095 0.7746 0.046 Uiso 1 1 calc R . .
C18 C 0.35279(17) 0.08417(16) 0.77218(8) 0.0236(4) Uani 1 1 d . . .
N20 N 0.38172(14) 0.16388(14) 0.72075(7) 0.0246(3) Uani 1 1 d . . .
H20 H 0.4566 0.2122 0.7141 0.030 Uiso 1 1 calc R . .
C21 C 0.30221(15) 0.17516(15) 0.67773(8) 0.0203(3) Uani 1 1 d . . .
C22 C 0.35001(15) 0.23335(14) 0.61703(7) 0.0175(3) Uani 1 1 d . . .
H22 H 0.4291 0.2568 0.6071 0.021 Uiso 1 1 calc R . .
N23 N 0.28676(12) 0.25680(12) 0.57248(6) 0.0156(2) Uani 1 1 d . . .
C24 C 0.17018(15) 0.21590(15) 0.58439(8) 0.0186(3) Uani 1 1 d . . .
H24 H 0.1247 0.2280 0.5525 0.022 Uiso 1 1 calc R . .
C25 C 0.11646(16) 0.15582(16) 0.64348(9) 0.0226(4) Uani 1 1 d . . .
H25 H 0.0357 0.1281 0.6508 0.027 Uiso 1 1 calc R . .
C26 C 0.18312(16) 0.13703(16) 0.69166(8) 0.0235(3) Uani 1 1 d . . .
H26 H 0.1489 0.0999 0.7322 0.028 Uiso 1 1 calc R . .
O27 O 0.37489(12) 0.68746(14) 0.97706(7) 0.0301(3) Uani 1 1 d . . .
O19 O 0.25163(12) 0.01458(12) 0.79023(6) 0.0292(3) Uani 1 1 d . . .
H27A H 0.329(3) 0.651(2) 1.0155(13) 0.044(7) Uiso 1 1 d . . .
H27B H 0.332(3) 0.706(3) 0.9427(15) 0.063(9) Uiso 1 1 d . . .


_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 N23 2.0276(13) 2_655 ?
Cu1 N23 2.0276(13) 6_656 ?
Cu1 N1 2.0438(13) 5_557 ?
Cu1 N1 2.0438(13) . ?
N1 C6 1.344(2) . ?
N1 C2 1.3463(19) . ?
C2 C3 1.386(2) . ?
C2 H2 0.9300 . ?
C3 C4 1.394(3) . ?
C3 C7 1.498(2) . ?
C4 C5 1.377(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.386(2) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 O8 1.234(2) . ?
C7 N9 1.341(2) . ?
N9 C10 1.454(2) . ?
N9 H9 0.8600 . ?
C10 C11 1.531(3) . ?
C10 C18 1.536(2) . ?
C10 H10 0.9800 . ?
C11 C12 1.498(3) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C17 1.383(3) . ?
C12 C13 1.390(3) . ?
C13 C14 1.372(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.380(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.382(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.385(3) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 O19 1.213(2) . ?
C18 N20 1.366(2) . ?
N20 C21 1.401(2) . ?
N20 H20 0.8600 . ?
C21 C26 1.389(2) . ?
C21 C22 1.395(2) . ?
C22 N23 1.340(2) . ?
C22 H22 0.9300 . ?
N23 C24 1.345(2) . ?
N23 Cu1 2.0276(13) 3_664 ?
C24 C25 1.390(2) . ?
C24 H24 0.9300 . ?
C25 C26 1.390(2) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
O27 H27A 0.94(3) . ?
O27 H27B 0.98(3) . ?

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
N23 Cu1 N23 94.02(8) 2_655 6_656 ?
N23 Cu1 N1 88.88(5) 2_655 5_557 ?
N23 Cu1 N1 176.57(6) 6_656 5_557 ?
N23 Cu1 N1 176.57(6) 2_655 . ?
N23 Cu1 N1 88.88(5) 6_656 . ?
N1 Cu1 N1 88.29(7) 5_557 . ?
C6 N1 C2 118.54(14) . . ?
C6 N1 Cu1 120.11(11) . . ?
C2 N1 Cu1 121.16(11) . . ?
N1 C2 C3 122.44(15) . . ?
N1 C2 H2 118.8 . . ?
C3 C2 H2 118.8 . . ?
C2 C3 C4 118.29(14) . . ?
C2 C3 C7 118.06(14) . . ?
C4 C3 C7 123.64(14) . . ?
C5 C4 C3 119.45(15) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 118.89(16) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
N1 C6 C5 122.30(15) . . ?
N1 C6 H6 118.8 . . ?
C5 C6 H6 118.8 . . ?
O8 C7 N9 124.00(15) . . ?
O8 C7 C3 121.13(14) . . ?
N9 C7 C3 114.86(14) . . ?
C7 N9 C10 122.34(14) . . ?
C7 N9 H9 118.8 . . ?
C10 N9 H9 118.8 . . ?
N9 C10 C11 111.48(14) . . ?
N9 C10 C18 109.21(14) . . ?
C11 C10 C18 107.69(14) . . ?
N9 C10 H10 109.5 . . ?
C11 C10 H10 109.5 . . ?
C18 C10 H10 109.5 . . ?
C12 C11 C10 117.58(15) . . ?
C12 C11 H11A 107.9 . . ?
C10 C11 H11A 107.9 . . ?
C12 C11 H11B 107.9 . . ?
C10 C11 H11B 107.9 . . ?
H11A C11 H11B 107.2 . . ?
C17 C12 C13 117.4(2) . . ?
C17 C12 C11 122.13(19) . . ?
C13 C12 C11 119.93(19) . . ?
C14 C13 C12 121.4(2) . . ?
C14 C13 H13 119.3 . . ?
C12 C13 H13 119.3 . . ?
C13 C14 C15 120.7(2) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
C14 C15 C16 118.6(2) . . ?
C14 C15 H15 120.7 . . ?
C16 C15 H15 120.7 . . ?
C15 C16 C17 120.4(3) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C12 C17 C16 121.3(2) . . ?
C12 C17 H17 119.3 . . ?
C16 C17 H17 119.3 . . ?
O19 C18 N20 124.65(17) . . ?
O19 C18 C10 123.41(15) . . ?
N20 C18 C10 111.85(15) . . ?
C18 N20 C21 126.83(16) . . ?
C18 N20 H20 116.6 . . ?
C21 N20 H20 116.6 . . ?
C26 C21 C22 118.56(15) . . ?
C26 C21 N20 125.51(15) . . ?
C22 C21 N20 115.90(15) . . ?
N23 C22 C21 122.73(15) . . ?
N23 C22 H22 118.6 . . ?
C21 C22 H22 118.6 . . ?
C22 N23 C24 118.95(13) . . ?
C22 N23 Cu1 117.45(11) . 3_664 ?
C24 N23 Cu1 122.51(11) . 3_664 ?
N23 C24 C25 121.16(15) . . ?
N23 C24 H24 119.4 . . ?
C25 C24 H24 119.4 . . ?
C26 C25 C24 120.19(16) . . ?
C26 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C21 C26 C25 118.24(15) . . ?
C21 C26 H26 120.9 . . ?
C25 C26 H26 120.9 . . ?
H27A O27 H27B 114(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N9 H9 Cl1 0.86 2.45 3.2865(15) 165.8 4_547
N20 H20 O27 0.86 1.96 2.815(2) 173.6 6_656
O27 H27A O8 0.94(3) 1.95(3) 2.8486(19) 159(2) 4_557
O27 H27B Cl1 0.98(3) 2.18(3) 3.1592(15) 175(2) 4_557

_diffrn_measured_fraction_theta_max 0.951
_diffrn_reflns_theta_full        32.02
_diffrn_measured_fraction_theta_full 0.951
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.070

# Attachment 'MOF 2 sb0387c_FINAL_R1.cif'

data_sb0387c
_database_code_depnum_ccdc_archive 'CCDC 699626'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H28 Cl Cu N8 O4'
_chemical_formula_weight         639.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           TETRAGONAL
_symmetry_space_group_name_H-M   P4

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'

_cell_length_a                   13.266(4)
_cell_length_b                   13.266(4)
_cell_length_c                   5.3885(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     948.3(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       NEEDLE
_exptl_crystal_colour            BLUE
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.120
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             330
_exptl_absorpt_coefficient_mu    0.684
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.8754
_exptl_absorpt_correction_T_max  0.9601
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER CCD AREA DETECTOR'
_diffrn_measurement_method       'OMEGA SCAN'
_diffrn_detector_area_resol_mean 3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7648
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_theta_min         1.54
_diffrn_reflns_theta_max         23.26
_reflns_number_total             1333
_reflns_number_gt                1276
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER AXS SMART 3'
_computing_cell_refinement       'BRUKER AXS SMART 3'
_computing_data_reduction        'BRUKER AXS SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'BRUKER SHELXTL'
_computing_publication_material  MERCURY1.4.2

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. The ligand backbone was found
to be disordered over a 2-fold axis. As a consequence, both N7 and C7 occupy
same site. EADP and EXYZ were used to keep these atoms on the same site. DFIX
and FLAT restraints were used to keep the bond distances and planarity of the
disordered backbone of the ligand.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1314P)²+5.3102P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(6)
_refine_ls_number_reflns         1333
_refine_ls_number_parameters     86
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0869
_refine_ls_wR_factor_ref         0.2339
_refine_ls_wR_factor_gt          0.2310
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.128
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 1.0000 1.0000 0.3666(3) 0.0187(6) Uani 1 4 d S . .
Cl1 Cl 1.0000 1.0000 -0.1025(11) 0.0259(12) Uani 1 4 d S . .
N1 N 0.9258(5) 0.8657(5) 0.3906(18) 0.0249(17) Uani 1 1 d . . .
C2 C 0.8483(7) 0.8434(7) 0.238(2) 0.033(2) Uani 1 1 d . . .
H2 H 0.8310 0.8882 0.1121 0.039 Uiso 1 1 calc R . .
C3 C 0.7948(9) 0.7555(10) 0.265(3) 0.056(3) Uani 1 1 d . . .
H3 H 0.7395 0.7433 0.1627 0.067 Uiso 1 1 calc R . .
C4 C 0.8215(11) 0.6858(10) 0.438(3) 0.068(4) Uani 1 1 d . . .
H4 H 0.7859 0.6258 0.4554 0.082 Uiso 1 1 calc R . .
C5 C 0.9035(10) 0.7074(8) 0.5893(19) 0.044(3) Uani 1 1 d . . .
C6 C 0.9544(8) 0.7981(7) 0.5579(18) 0.031(2) Uani 1 1 d . . .
H6 H 1.0101 0.8118 0.6570 0.037 Uiso 1 1 calc R . .
N7 N 0.9342(11) 0.6378(9) 0.768(3) 0.085(4) Uiso 0.50 1 d PD . .
C7 C 0.9342(11) 0.6378(9) 0.768(3) 0.085(4) Uiso 0.50 1 d PD . .
O8 O 1.0196(14) 0.652(2) 0.838(7) 0.118(8) Uiso 0.50 1 d PD . .
N9 N 0.9252(9) 0.5460(9) 0.848(4) 0.036(3) Uiso 0.50 1 d PD . .
O11 O 1.0751(9) 0.6734(8) 0.823(3) 0.032(3) Uiso 0.50 1 d PD . .
C12 C 1.0000 0.5000 1.008(4) 0.106(9) Uiso 1 2 d SD . .
C13 C 1.076(2) 0.542(2) 1.206(5) 0.079(9) Uiso 0.50 1 d PD . .
C10 C 1.0167(11) 0.6055(9) 0.881(4) 0.068 Uiso 0.50 1 d PD . .


_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 N1 2.040(6) 4_575 ?
Cu1 N1 2.040(6) 2_755 ?
Cu1 N1 2.040(6) . ?
Cu1 N1 2.040(6) 3_775 ?
Cu1 Cl1 2.528(6) . ?
N1 C6 1.326(13) . ?
N1 C2 1.350(13) . ?
C2 C3 1.373(17) . ?
C3 C4 1.362(19) . ?
C4 C5 1.388(19) . ?
C5 N7 1.395(16) . ?
C5 C6 1.391(15) . ?
N7 O8 1.209(10) . ?
N7 N9 1.298(9) . ?
N7 C10 1.325(10) . ?
O8 C10 0.66(3) . ?
O8 O11 0.79(2) . ?
O8 N9 1.89(3) . ?
N9 C10 1.460(19) . ?
N9 C12 1.448(10) . ?
O11 C10 1.229(9) . ?
C12 N9 1.448(10) 3_765 ?
C12 C13 1.568(10) 3_765 ?
C12 C13 1.568(10) . ?
C12 C10 1.573(9) . ?
C12 C10 1.573(9) 3_765 ?

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
N1 Cu1 N1 172.7(6) 4_575 2_755 ?
N1 Cu1 N1 89.77(4) 4_575 . ?
N1 Cu1 N1 89.77(4) 2_755 . ?
N1 Cu1 N1 89.77(4) 4_575 3_775 ?
N1 Cu1 N1 89.77(4) 2_755 3_775 ?
N1 Cu1 N1 172.7(6) . 3_775 ?
N1 Cu1 Cl1 93.6(3) 4_575 . ?
N1 Cu1 Cl1 93.6(3) 2_755 . ?
N1 Cu1 Cl1 93.6(3) . . ?
N1 Cu1 Cl1 93.6(3) 3_775 . ?
C6 N1 C2 119.0(7) . . ?
C6 N1 Cu1 119.7(7) . . ?
C2 N1 Cu1 121.3(7) . . ?
N1 C2 C3 121.0(10) . . ?
C2 C3 C4 120.9(12) . . ?
C3 C4 C5 117.8(10) . . ?
N7 C5 C6 121.0(12) . . ?
N7 C5 C4 119.8(11) . . ?
C6 C5 C4 119.2(10) . . ?
N1 C6 C5 121.9(10) . . ?
O8 N7 N9 97.6(17) . . ?
O8 N7 C5 112.5(19) . . ?
N9 N7 C5 145.5(14) . . ?
N9 N7 C10 67.7(10) . . ?
C5 N7 C10 140.7(13) . . ?
C10 O8 O11 115(3) . . ?
C10 O8 N7 84.8(17) . . ?
O11 O8 N7 154(5) . . ?
O11 O8 N9 152(3) . . ?
N7 N9 C10 57.1(7) . . ?
N7 N9 C12 122.0(11) . . ?
C10 N9 C12 65.5(7) . . ?
C12 N9 O8 83.0(10) . . ?
N9 C12 N9 107.2(18) . 3_765 ?
N9 C12 C13 96.5(14) . 3_765 ?
N9 C12 C13 134.1(13) 3_765 3_765 ?
N9 C12 C13 134.1(13) . . ?
N9 C12 C13 96.5(14) 3_765 . ?
C13 C12 C13 94(3) 3_765 . ?
N9 C12 C10 57.6(8) . . ?
N9 C12 C10 91.2(11) 3_765 . ?
C13 C12 C10 134.4(14) 3_765 . ?
C13 C12 C10 83.7(13) . . ?
N9 C12 C10 91.2(11) . 3_765 ?
N9 C12 C10 57.6(8) 3_765 3_765 ?
C13 C12 C10 83.7(13) 3_765 3_765 ?
C13 C12 C10 134.4(14) . 3_765 ?
C10 C12 C10 128.7(17) . 3_765 ?
O8 C10 N9 120.6(15) . . ?
O11 C10 N9 152.9(13) . . ?
O8 C10 N7 65.3(12) . . ?
O11 C10 N7 99.6(11) . . ?
N9 C10 N7 55.3(7) . . ?
O8 C10 C12 173(4) . . ?
O11 C10 C12 148.4(13) . . ?
N9 C10 C12 56.9(5) . . ?
N7 C10 C12 111.7(10) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        23.26
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.964
_refine_diff_density_min         -1.045
_refine_diff_density_rms         0.127


