# Electronic Supplementary Material (ESI) 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        'Hongbin Du'
_publ_contact_author_email       HBDU@NJU.EDU.CN

_publ_section_title              
;
A Photoluminscent Interpenetrating Diamondoid
Metal-Organic Framework Based on Cu4I4 Clusters with High
Thermal Stability
;
loop_
_publ_author_name
'Hongbin Du'
'Yi-Zhi Li'
'Shi-Bin Ren'
'Xiao-Zeng You'
'Jun Zhang'
'Le Zhou'

# Attachment '281113E_0m.cif'

data_281113e_0m
_database_code_depnum_ccdc_archive 'CCDC 725250'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C25 H24 Cu4 I4 N4 O4, H2 O'
_chemical_formula_sum            'C25 H26 Cu4 I4 N4 O5'
_chemical_melting_point          ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?

_diffrn_ambient_temperature      291(2)
_chemical_formula_weight         1224.26

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'
I I -0.4742 1.8119 '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 -4'
_symmetry_int_tables_number      82
_chemical_absolute_configuration ?
_symmetry_space_group_name_Hall  'I -4 '

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

_cell_length_a                   13.3852(8)
_cell_length_b                   13.3852(8)
_cell_length_c                   9.9922(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1790.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    2049
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      24.11
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1144
_exptl_absorpt_coefficient_mu    5.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.291
_exptl_absorpt_correction_T_max  0.354
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
;
?
;
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Aepex CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4939
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         26.00
_reflns_number_total             1757
_reflns_number_gt                1603
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       'SMART '
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_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)+(0.06P)²+1.99P] 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   0.05(6)
_refine_ls_number_reflns         1757
_refine_ls_number_parameters     95
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0448
_refine_ls_wR_factor_ref         0.1027
_refine_ls_wR_factor_gt          0.1016
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_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
C1 C 1.0000 0.5000 0.2500 0.034(4) Uani 1 4 d S . .
C2 C 0.9054(8) 0.5273(8) 0.3336(9) 0.040(2) Uani 1 1 d . . .
H2A H 0.9168 0.5879 0.3846 0.048 Uiso 1 1 calc R . .
H2B H 0.8484 0.5376 0.2753 0.048 Uiso 1 1 calc R . .
C3 C 0.8200(8) 0.4567(7) 0.5192(9) 0.037(2) Uani 1 1 d . . .
C4 C 0.7641(8) 0.5420(8) 0.5327(10) 0.042(2) Uani 1 1 d . . .
H4 H 0.7709 0.5945 0.4724 0.050 Uiso 1 1 calc R . .
C5 C 0.6965(8) 0.5481(8) 0.6393(11) 0.043(2) Uani 1 1 d . . .
H5 H 0.6576 0.6051 0.6494 0.051 Uiso 1 1 calc R . .
C6 C 0.7414(8) 0.3854(8) 0.7117(9) 0.037(2) Uani 1 1 d . . .
H6 H 0.7312 0.3316 0.7691 0.045 Uiso 1 1 calc R . .
C7 C 0.8115(7) 0.3770(7) 0.6106(10) 0.041(2) Uani 1 1 d . . .
H7 H 0.8517 0.3206 0.6032 0.049 Uiso 1 1 calc R . .
Cu1 Cu 0.59499(8) 0.48717(8) 0.89163(12) 0.0361(3) Uani 1 1 d . . .
I1 I 0.52815(4) 0.67667(4) 0.87166(6) 0.03868(18) Uani 1 1 d . . .
N1 N 0.6868(6) 0.4706(6) 0.7296(7) 0.0362(15) Uani 1 1 d . . .
O1 O 0.8880(5) 0.4448(5) 0.4214(7) 0.0401(16) Uani 1 1 d . . .
O1W O 0.0000 0.5000 0.7500 0.049(4) Uani 1 4 d S . .
H1WA H 0.0575 0.4833 0.7784 0.059 Uiso 0.25 1 d PR . .
H1WB H -0.0143 0.5581 0.7784 0.059 Uiso 0.25 1 d PR . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.038(6) 0.038(6) 0.028(9) 0.000 0.000 0.000
C2 0.043(5) 0.052(6) 0.024(4) 0.002(4) 0.015(4) -0.002(4)
C3 0.054(6) 0.033(5) 0.025(4) -0.006(4) 0.002(4) -0.004(4)
C4 0.048(5) 0.043(5) 0.034(5) -0.001(4) 0.004(4) 0.001(4)
C5 0.051(5) 0.048(5) 0.029(5) -0.001(4) 0.004(5) 0.003(4)
C6 0.042(5) 0.040(5) 0.030(4) -0.006(4) 0.004(4) -0.005(4)
C7 0.051(5) 0.044(5) 0.027(4) -0.001(4) 0.007(5) -0.001(4)
Cu1 0.0364(5) 0.0375(6) 0.0343(6) 0.0045(5) 0.0048(5) 0.0082(4)
I1 0.0386(3) 0.0377(3) 0.0398(3) 0.0045(3) 0.0049(3) 0.0069(2)
N1 0.036(4) 0.039(4) 0.033(4) -0.007(3) 0.000(3) -0.008(3)
O1 0.032(3) 0.042(4) 0.047(4) 0.007(3) 0.004(3) 0.004(3)
O1W 0.051(5) 0.051(5) 0.044(9) 0.000 0.000 0.000

_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
C1 C2 1.560(9) 8_645 ?
C1 C2 1.560(9) 2_765 ?
C1 C2 1.560(9) . ?
C1 C2 1.560(9) 7_565 ?
C2 O1 1.429(12) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 O1 1.345(11) . ?
C3 C4 1.372(14) . ?
C3 C7 1.408(14) . ?
C4 C5 1.399(14) . ?
C4 H4 0.9300 . ?
C5 N1 1.380(13) . ?
C5 H5 0.9300 . ?
C6 N1 1.367(14) . ?
C6 C7 1.383(14) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
Cu1 N1 2.045(8) . ?
Cu1 Cu1 2.566(2) 2_665 ?
Cu1 I1 2.6138(13) 3_567 ?
Cu1 I1 2.6970(12) . ?
Cu1 I1 2.7507(13) 2_665 ?
Cu1 Cu1 2.825(2) 3_567 ?
Cu1 Cu1 2.825(2) 4_657 ?
I1 Cu1 2.6138(13) 4_657 ?
I1 Cu1 2.7507(13) 2_665 ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8500 . ?

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
C2 C1 C2 106.7(3) 8_645 2_765 ?
C2 C1 C2 106.7(3) 8_645 . ?
C2 C1 C2 115.2(7) 2_765 . ?
C2 C1 C2 115.2(7) 8_645 7_565 ?
C2 C1 C2 106.7(3) 2_765 7_565 ?
C2 C1 C2 106.7(3) . 7_565 ?
O1 C2 C1 106.3(7) . . ?
O1 C2 H2A 110.5 . . ?
C1 C2 H2A 110.5 . . ?
O1 C2 H2B 110.5 . . ?
C1 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
O1 C3 C4 122.6(9) . . ?
O1 C3 C7 115.9(9) . . ?
C4 C3 C7 121.5(9) . . ?
C3 C4 C5 118.4(10) . . ?
C3 C4 H4 120.8 . . ?
C5 C4 H4 120.8 . . ?
N1 C5 C4 121.0(9) . . ?
N1 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
N1 C6 C7 121.7(9) . . ?
N1 C6 H6 119.1 . . ?
C7 C6 H6 119.1 . . ?
C6 C7 C3 117.8(9) . . ?
C6 C7 H7 121.1 . . ?
C3 C7 H7 121.1 . . ?
N1 Cu1 Cu1 127.6(2) . 2_665 ?
N1 Cu1 I1 117.2(2) . 3_567 ?
Cu1 Cu1 I1 115.15(3) 2_665 3_567 ?
N1 Cu1 I1 104.0(2) . . ?
Cu1 Cu1 I1 62.96(4) 2_665 . ?
I1 Cu1 I1 106.23(4) 3_567 . ?
N1 Cu1 I1 102.5(2) . 2_665 ?
Cu1 Cu1 I1 60.85(5) 2_665 2_665 ?
I1 Cu1 I1 104.70(4) 3_567 2_665 ?
I1 Cu1 I1 123.07(4) . 2_665 ?
N1 Cu1 Cu1 150.7(2) . 3_567 ?
Cu1 Cu1 Cu1 62.99(2) 2_665 3_567 ?
I1 Cu1 Cu1 59.30(5) 3_567 3_567 ?
I1 Cu1 Cu1 104.68(4) . 3_567 ?
I1 Cu1 Cu1 55.89(3) 2_665 3_567 ?
N1 Cu1 Cu1 153.7(2) . 4_657 ?
Cu1 Cu1 Cu1 62.99(2) 2_665 4_657 ?
I1 Cu1 Cu1 60.61(5) 3_567 4_657 ?
I1 Cu1 Cu1 56.44(3) . 4_657 ?
I1 Cu1 Cu1 103.27(4) 2_665 4_657 ?
Cu1 Cu1 Cu1 54.01(5) 3_567 4_657 ?
Cu1 I1 Cu1 64.26(5) 4_657 . ?
Cu1 I1 Cu1 63.50(4) 4_657 2_665 ?
Cu1 I1 Cu1 56.19(4) . 2_665 ?
C6 N1 C5 119.4(8) . . ?
C6 N1 Cu1 121.0(6) . . ?
C5 N1 Cu1 119.5(7) . . ?
C3 O1 C2 117.7(7) . . ?
H1WA O1W H1WB 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
C2 C1 C2 O1 63.0(4) 8_645 . . . ?
C2 C1 C2 O1 -55.1(5) 2_765 . . . ?
C2 C1 C2 O1 -173.3(8) 7_565 . . . ?
O1 C3 C4 C5 -178.8(9) . . . . ?
C7 C3 C4 C5 -0.8(16) . . . . ?
C3 C4 C5 N1 0.6(16) . . . . ?
N1 C6 C7 C3 -4.7(15) . . . . ?
O1 C3 C7 C6 -179.1(8) . . . . ?
C4 C3 C7 C6 2.8(15) . . . . ?
N1 Cu1 I1 Cu1 -160.5(2) . . . 4_657 ?
Cu1 Cu1 I1 Cu1 74.14(3) 2_665 . . 4_657 ?
I1 Cu1 I1 Cu1 -36.25(4) 3_567 . . 4_657 ?
I1 Cu1 I1 Cu1 84.08(5) 2_665 . . 4_657 ?
Cu1 Cu1 I1 Cu1 25.50(5) 3_567 . . 4_657 ?
N1 Cu1 I1 Cu1 125.3(2) . . . 2_665 ?
I1 Cu1 I1 Cu1 -110.39(3) 3_567 . . 2_665 ?
I1 Cu1 I1 Cu1 9.93(6) 2_665 . . 2_665 ?
Cu1 Cu1 I1 Cu1 -48.65(5) 3_567 . . 2_665 ?
Cu1 Cu1 I1 Cu1 -74.14(3) 4_657 . . 2_665 ?
C7 C6 N1 C5 4.5(14) . . . . ?
C7 C6 N1 Cu1 -173.2(7) . . . . ?
C4 C5 N1 C6 -2.3(15) . . . . ?
C4 C5 N1 Cu1 175.4(8) . . . . ?
Cu1 Cu1 N1 C6 -118.8(7) 2_665 . . . ?
I1 Cu1 N1 C6 57.8(7) 3_567 . . . ?
I1 Cu1 N1 C6 174.7(7) . . . . ?
I1 Cu1 N1 C6 -56.1(7) 2_665 . . . ?
Cu1 Cu1 N1 C6 -17.2(10) 3_567 . . . ?
Cu1 Cu1 N1 C6 135.9(6) 4_657 . . . ?
Cu1 Cu1 N1 C5 63.5(8) 2_665 . . . ?
I1 Cu1 N1 C5 -119.9(7) 3_567 . . . ?
I1 Cu1 N1 C5 -3.0(8) . . . . ?
I1 Cu1 N1 C5 126.1(7) 2_665 . . . ?
Cu1 Cu1 N1 C5 165.1(5) 3_567 . . . ?
Cu1 Cu1 N1 C5 -41.8(10) 4_657 . . . ?
C4 C3 O1 C2 3.5(14) . . . . ?
C7 C3 O1 C2 -174.5(9) . . . . ?
C1 C2 O1 C3 169.5(7) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.143


