# 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        'Jie Zhang'
_publ_contact_author_email       ZHANGJIE@FJIRSM.AC.CN

_publ_section_title              
;
An unprecdented 9-fold [3 3] interpenetrated diamondoid
network coordination polymer containing Cu(II)-based "paddlewheels" as
connecting node
;
loop_
_publ_author_name
'Jie Zhang'
'Xu-Hui Jin'
'Zhan-Feng Ju'
'Qing-Xia Yao'
'Hai-Xia Zhang'

# Attachment 'cif-ZHX-CECB903214B-R.txt'

data_1:
_database_code_depnum_ccdc_archive 'CCDC 720013'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '[Cu2C52H40N6O14] 0.5Cl 0.5(OH) 8H2O'
_chemical_formula_sum            'C52 H56.50 Cl0.50 Cu2 N6 O22.50'
_chemical_formula_weight         1270.34

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'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   I-42d

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'x, -y+1/2, -z+1/4'
'-x, y+1/2, -z+1/4'
'-y, -x+1/2, z+1/4'
'y, x+1/2, z+1/4'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1, -z+3/4'
'-x+1/2, y+1, -z+3/4'
'-y+1/2, -x+1, z+3/4'
'y+1/2, x+1, z+3/4'

_cell_length_a                   13.335(2)
_cell_length_b                   13.335(2)
_cell_length_c                   31.626(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5624.2(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7273
_cell_measurement_theta_min      2.1609
_cell_measurement_theta_max      27.4797

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.6000
_exptl_crystal_size_mid          0.3000
_exptl_crystal_size_min          0.3000
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2628
_exptl_absorpt_coefficient_mu    0.866
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8094
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   '(R.H. Blessing, 1995&1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  'CCD area detector'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20911
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         2.51
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3221
_reflns_number_gt                3077
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.1349P)²+2.4181P] 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   0.00(3)
_refine_ls_number_reflns         3221
_refine_ls_number_parameters     178
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0674
_refine_ls_wR_factor_ref         0.1980
_refine_ls_wR_factor_gt          0.1942
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.000
_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 0.5000 0.5000 0.045555(19) 0.0470(2) Uani 1 2 d S . .
O1 O 0.3642(2) 0.4521(2) 0.04568(10) 0.0584(7) Uani 1 1 d . . .
O2 O 0.3613(2) 0.4499(2) -0.02560(9) 0.0578(7) Uani 1 1 d . . .
O3 O 0.4783(5) 0.5660(6) 0.1128(2) 0.134(2) Uani 1 1 d . . .
O4 O 0.5000 0.5000 0.17237(19) 0.145(4) Uani 1 2 d S . .
N1 N 0.5000 0.5000 0.13457(19) 0.0727(15) Uani 1 2 d S . .
N2 N -0.1333(2) 0.2840(3) -0.02643(11) 0.0542(8) Uani 1 1 d . . .
C1 C 0.3227(3) 0.4357(3) 0.01048(13) 0.0499(8) Uani 1 1 d . . .
C2 C 0.2182(3) 0.3964(3) 0.01204(12) 0.0473(7) Uani 1 1 d . . .
C3 C 0.1572(3) 0.4128(3) 0.04694(14) 0.0525(8) Uani 1 1 d . . .
H3A H 0.1826 0.4465 0.0703 0.063 Uiso 1 1 calc R . .
C4 C 0.0575(3) 0.3790(3) 0.04724(13) 0.0538(8) Uani 1 1 d . . .
H4A H 0.0161 0.3934 0.0701 0.065 Uiso 1 1 calc R . .
C5 C 0.0211(3) 0.3245(3) 0.01354(12) 0.0530(8) Uani 1 1 d . . .
C6 C 0.0829(3) 0.3055(4) -0.02133(13) 0.0595(10) Uani 1 1 d . . .
H6A H 0.0591 0.2676 -0.0439 0.071 Uiso 1 1 calc R . .
C7 C 0.1797(3) 0.3434(3) -0.02210(14) 0.0546(9) Uani 1 1 d . . .
H7A H 0.2195 0.3332 -0.0459 0.066 Uiso 1 1 calc R . .
C8 C -0.0832(3) 0.2826(5) 0.01542(13) 0.0662(12) Uani 1 1 d . . .
H8A H -0.0805 0.2142 0.0257 0.079 Uiso 1 1 calc R . .
H8B H -0.1226 0.3216 0.0353 0.079 Uiso 1 1 calc R . .
C9 C -0.1730(3) 0.3699(4) -0.04060(16) 0.0610(10) Uani 1 1 d . . .
H9A H -0.1688 0.4274 -0.0240 0.073 Uiso 1 1 calc R . .
C10 C -0.2200(3) 0.3747(3) -0.07940(15) 0.0557(9) Uani 1 1 d . . .
H10A H -0.2487 0.4343 -0.0887 0.067 Uiso 1 1 calc R . .
C11 C -0.2238(3) 0.2892(3) -0.10430(13) 0.0469(8) Uani 1 1 d . . .
C12 C -0.1802(3) 0.2009(3) -0.08894(15) 0.0543(9) Uani 1 1 d . . .
H12A H -0.1808 0.1428 -0.1052 0.065 Uiso 1 1 calc R . .
C13 C -0.1364(3) 0.2007(3) -0.04958(14) 0.0543(9) Uani 1 1 d . . .
H13A H -0.1086 0.1418 -0.0390 0.065 Uiso 1 1 calc R . .
Cl Cl 0.0000 0.0000 0.0000 0.0724(8) Uiso 0.50 4 d SP . .
OH1 O 0.0000 0.0000 0.0000 0.0724(8) Uiso 0.50 4 d SP . .
O2W O -0.2492(13) 0.3509(11) 0.1079(5) 0.241(6) Uiso 1 1 d . . .
O1W O -0.0705(19) 0.1190(18) 0.0977(8) 0.342(11) 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 O1 1.920(3) 3_665 ?
Cu1 O1 1.920(3) . ?
Cu1 O2 2.065(3) 4_655 ?
Cu1 O2 2.065(3) 2_565 ?
Cu1 O3 2.321(9) 3_665 ?
Cu1 O3 2.321(9) . ?
Cu1 Cu1 2.8815(14) 2_565 ?
O1 C1 1.262(5) . ?
O2 C1 1.266(5) . ?
O2 Cu1 2.065(3) 2_565 ?
O3 N1 1.153(7) . ?
O4 N1 1.196(9) . ?
N1 O3 1.153(7) 3_665 ?
N2 C13 1.331(6) . ?
N2 C9 1.340(6) . ?
N2 C8 1.482(5) . ?
C1 C2 1.489(5) . ?
C2 C3 1.389(6) . ?
C2 C7 1.389(6) . ?
C3 C4 1.403(6) . ?
C4 C5 1.379(6) . ?
C5 C6 1.399(6) . ?
C5 C8 1.501(5) . ?
C6 C7 1.387(6) . ?
C9 C10 1.380(7) . ?
C10 C11 1.386(6) . ?
C11 C12 1.400(6) . ?
C11 C11 1.484(8) 14_444 ?
C12 C13 1.375(6) . ?

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 179.77(19) 3_665 . ?
O1 Cu1 O2 89.63(13) 3_665 4_655 ?
O1 Cu1 O2 90.44(14) . 4_655 ?
O1 Cu1 O2 90.44(14) 3_665 2_565 ?
O1 Cu1 O2 89.63(13) . 2_565 ?
O2 Cu1 O2 144.41(17) 4_655 2_565 ?
O1 Cu1 O3 90.37(19) 3_665 3_665 ?
O1 Cu1 O3 89.43(19) . 3_665 ?
O2 Cu1 O3 84.28(19) 4_655 3_665 ?
O2 Cu1 O3 131.30(19) 2_565 3_665 ?
O1 Cu1 O3 89.43(19) 3_665 . ?
O1 Cu1 O3 90.37(19) . . ?
O2 Cu1 O3 131.30(19) 4_655 . ?
O2 Cu1 O3 84.28(19) 2_565 . ?
O3 Cu1 O3 47.0(3) 3_665 . ?
O1 Cu1 Cu1 90.11(9) 3_665 2_565 ?
O1 Cu1 Cu1 90.11(9) . 2_565 ?
O2 Cu1 Cu1 72.21(8) 4_655 2_565 ?
O2 Cu1 Cu1 72.21(8) 2_565 2_565 ?
O3 Cu1 Cu1 156.48(17) 3_665 2_565 ?
O3 Cu1 Cu1 156.48(17) . 2_565 ?
C1 O1 Cu1 118.0(3) . . ?
C1 O2 Cu1 133.5(3) . 2_565 ?
N1 O3 Cu1 103.1(6) . . ?
O3 N1 O3 106.8(10) . 3_665 ?
O3 N1 O4 126.6(5) . . ?
O3 N1 O4 126.6(5) 3_665 . ?
C13 N2 C9 121.2(4) . . ?
C13 N2 C8 119.6(4) . . ?
C9 N2 C8 119.2(4) . . ?
O1 C1 O2 126.2(3) . . ?
O1 C1 C2 116.2(3) . . ?
O2 C1 C2 117.6(3) . . ?
C3 C2 C7 118.8(3) . . ?
C3 C2 C1 121.3(3) . . ?
C7 C2 C1 119.9(3) . . ?
C2 C3 C4 120.7(4) . . ?
C5 C4 C3 119.8(4) . . ?
C4 C5 C6 119.8(3) . . ?
C4 C5 C8 119.5(4) . . ?
C6 C5 C8 120.7(4) . . ?
C7 C6 C5 119.7(4) . . ?
C6 C7 C2 121.1(4) . . ?
N2 C8 C5 112.2(3) . . ?
N2 C9 C10 121.1(4) . . ?
C9 C10 C11 119.0(4) . . ?
C10 C11 C12 118.6(4) . . ?
C10 C11 C11 121.2(3) . 14_444 ?
C12 C11 C11 120.1(3) . 14_444 ?
C13 C12 C11 119.5(4) . . ?
N2 C13 C12 120.6(4) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.699
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.117


