#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:23:22 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179662 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/15/4511504.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4511504
loop_
_publ_author_name
'Sarkar, Madhushree'
'Biradha, Kumar'
_publ_section_title
;
 Interplay of Hydrogen Bonds in Assembling (4,4)-Coordination
 Networks:  Transformations from Open to Interpenetrated Networks
 via Anion Exchange
;
_journal_issue                   8
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1742
_journal_paper_doi               10.1021/cg060216y
_journal_volume                  6
_journal_year                    2006
_chemical_formula_sum            'C34 H48 Cl2 Cu N8 O16'
_chemical_formula_weight         959.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           144
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31'
_symmetry_space_group_name_H-M   'P 31'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   17.943(3)
_cell_length_b                   17.943(3)
_cell_length_c                   13.252(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      8
_cell_volume                     3694.9(12)
_computing_cell_refinement       CAD4
_computing_data_collection       CAD4
_computing_data_reduction        CAD4
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       ω-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0122
_diffrn_reflns_av_sigmaI/netI    0.0616
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4699
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         1.31
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.620
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Hexagons
_exptl_crystal_F_000             1497
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.288
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         4684
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.288
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0767
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+3.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1895
_refine_ls_wR_factor_ref         0.2122
_reflns_number_gt                3752
_reflns_number_total             4684
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg060216ysi20060413_032804.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3694.9(10)
_cod_original_sg_symbol_H-M      P31
_cod_database_code               4511504
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
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
Cu1 Cu 0.73667(7) 2.06689(7) 0.35059(10) 0.0346(3) Uani 1 1 d .
O1W O 0.3305(5) 0.2618(5) 0.2055(7) 0.054(2) Uani 1 1 d .
O2W O 0.7267(6) 2.0566(6) 0.1715(6) 0.056(2) Uani 1 1 d .
N11A N 0.6992(7) 1.9397(6) 0.3588(8) 0.049(2) Uani 1 1 d .
O16A O 0.6541(9) 1.6712(7) 0.5247(9) 0.094(4) Uani 1 1 d .
C11A C 0.6671(8) 1.7719(6) 0.3967(10) 0.053(3) Uani 1 1 d .
C12A C 0.6317(8) 1.8109(8) 0.4611(11) 0.061(3) Uani 1 1 d .
H12A H 0.5974 1.7808 0.5159 0.074 Uiso 1 1 calc R
C13A C 0.6488(7) 1.8915(7) 0.4411(9) 0.049(3) Uani 1 1 d .
H13A H 0.6262 1.9165 0.4837 0.058 Uiso 1 1 calc R
C14A C 0.7320(8) 1.9048(8) 0.2963(9) 0.049(3) Uani 1 1 d .
H14A H 0.7671 1.9358 0.2424 0.059 Uiso 1 1 calc R
C15A C 0.7108(8) 1.8169(7) 0.3157(10) 0.053(3) Uani 1 1 d .
H15A H 0.7287 1.7902 0.2692 0.063 Uiso 1 1 calc R
C16A C 0.6535(11) 1.6851(8) 0.4275(10) 0.069(4) Uani 1 1 d .
N21A N 0.7747(5) 1.1954(5) 0.3485(7) 0.042(2) Uani 1 1 d .
O26A O 0.8891(6) 1.5080(5) 0.4172(7) 0.060(2) Uani 1 1 d .
C21A C 0.8237(9) 1.3666(7) 0.3469(10) 0.058(3) Uani 1 1 d .
C22A C 0.8608(7) 1.3365(6) 0.4095(8) 0.043(2) Uani 1 1 d .
H22A H 0.9046 1.3744 0.4522 0.052 Uiso 1 1 calc R
C23A C 0.8362(7) 1.2534(6) 0.4118(8) 0.044(3) Uani 1 1 d .
H23A H 0.8617 1.2342 0.4582 0.053 Uiso 1 1 calc R
C24A C 0.7338(7) 1.2236(6) 0.2880(8) 0.042(2) Uani 1 1 d .
H24A H 0.6877 1.1845 0.2489 0.050 Uiso 1 1 calc R
C25A C 0.7597(8) 1.3106(7) 0.2832(8) 0.047(2) Uani 1 1 d .
H25A H 0.7342 1.3305 0.2377 0.056 Uiso 1 1 calc R
C26A C 0.8535(8) 1.4645(7) 0.3474(9) 0.050(3) Uani 1 1 d .
N31A N 0.6410(8) 1.6314(7) 0.3551(9) 0.070(3) Uani 1 1 d .
H31A H 0.6354 1.6437 0.2939 0.084 Uiso 1 1 calc R
N32A N 0.8340(8) 1.4930(7) 0.2613(8) 0.068(3) Uani 1 1 d .
H32A H 0.8132 1.4585 0.2107 0.081 Uiso 1 1 calc R
C31A C 0.6363(10) 1.5462(7) 0.3801(13) 0.072(4) Uani 1 1 d .
H31B H 0.5957 1.5012 0.3357 0.087 Uiso 1 1 calc .
H31C H 0.6175 1.5298 0.4493 0.087 Uiso 1 1 calc .
C32A C 0.7322(10) 1.5598(9) 0.3647(12) 0.070(4) Uani 1 1 d .
H32B H 0.7715 1.6060 0.4088 0.084 Uiso 1 1 calc .
H32C H 0.7315 1.5078 0.3860 0.084 Uiso 1 1 calc .
C33A C 0.7641(10) 1.5791(8) 0.2668(10) 0.063(3) Uani 1 1 d .
H33A H 0.7732 1.6354 0.2488 0.076 Uiso 1 1 calc .
H33B H 0.7213 1.5375 0.2211 0.076 Uiso 1 1 calc .
C34A C 0.8469(10) 1.5787(9) 0.2522(10) 0.065(3) Uani 1 1 d .
H34A H 0.8701 1.6015 0.1860 0.079 Uiso 1 1 calc .
H34B H 0.8884 1.6157 0.3022 0.079 Uiso 1 1 calc .
N11B N 0.6091(5) 2.0323(5) 0.3527(7) 0.041(2) Uani 1 1 d .
O16B O 0.3274(6) 1.9748(8) 0.4735(9) 0.083(3) Uani 1 1 d .
C11B C 0.4371(8) 1.9809(9) 0.3733(10) 0.054(3) Uani 1 1 d .
C12B C 0.4980(7) 2.0473(7) 0.4295(10) 0.052(3) Uani 1 1 d .
H12B H 0.4816 2.0765 0.4741 0.063 Uiso 1 1 calc R
C13B C 0.5828(8) 2.0710(8) 0.4206(11) 0.058(3) Uani 1 1 d .
H13B H 0.6232 2.1144 0.4616 0.070 Uiso 1 1 calc R
C14B C 0.5540(6) 1.9756(7) 0.2988(9) 0.043(3) Uani 1 1 d .
H14B H 0.5735 1.9519 0.2504 0.052 Uiso 1 1 calc R
C15B C 0.4684(8) 1.9444(9) 0.3026(12) 0.072(4) Uani 1 1 d .
H15B H 0.4311 1.9002 0.2600 0.086 Uiso 1 1 calc R
C16B C 0.3470(8) 1.9566(8) 0.3951(10) 0.055(3) Uani 1 1 d .
N21B N -0.1399(5) 2.0938(6) 0.3524(6) 0.0367(19) Uani 1 1 d .
O26B O 0.1787(5) 2.2033(6) 0.3149(8) 0.068(3) Uani 1 1 d .
C21B C 0.0293(7) 2.1218(7) 0.3558(7) 0.040(2) Uani 1 1 d .
C22B C -0.0356(8) 2.0616(8) 0.4182(8) 0.051(3) Uani 1 1 d .
H22B H -0.0234 2.0281 0.4611 0.062 Uiso 1 1 calc R
C23B C -0.1150(7) 2.0510(7) 0.4178(7) 0.040(2) Uani 1 1 d .
H23B H -0.1551 2.0129 0.4639 0.048 Uiso 1 1 calc R
C24B C -0.0767(8) 2.1507(8) 0.2885(9) 0.054(3) Uani 1 1 d .
H24B H -0.0906 2.1811 0.2425 0.065 Uiso 1 1 calc R
C25B C 0.0055(9) 2.1648(7) 0.2892(9) 0.057(3) Uani 1 1 d .
H25B H 0.0458 2.2040 0.2442 0.068 Uiso 1 1 calc R
C26B C 0.1211(6) 2.1356(8) 0.3501(8) 0.047(3) Uani 1 1 d .
N31B N 0.2898(7) 1.9143(9) 0.3181(8) 0.072(3) Uani 1 1 d .
H31D H 0.3064 1.8972 0.2667 0.087 Uiso 1 1 calc R
N32B N 0.1303(6) 2.0695(7) 0.3824(9) 0.057(3) Uani 1 1 d .
H32D H 0.0855 2.0214 0.3979 0.069 Uiso 1 1 calc R
C31B C 0.2018(7) 1.8980(10) 0.3215(11) 0.066(4) Uani 1 1 d .
H31E H 0.1858 1.9004 0.3909 0.079 Uiso 1 1 calc .
H31F H 0.1630 1.8407 0.2957 0.079 Uiso 1 1 calc .
C32B C 0.1934(11) 1.9611(12) 0.2618(13) 0.083(5) Uani 1 1 d .
H32E H 0.1330 1.9445 0.2601 0.100 Uiso 1 1 calc .
H32F H 0.2104 1.9581 0.1931 0.100 Uiso 1 1 calc .
C33B C 0.2451(12) 2.0561(14) 0.2965(14) 0.095(6) Uani 1 1 d .
H33C H 0.3048 2.0711 0.3044 0.114 Uiso 1 1 calc .
H33D H 0.2431 2.0918 0.2429 0.114 Uiso 1 1 calc .
C34B C 0.2171(8) 2.0787(10) 0.3915(10) 0.064(3) Uani 1 1 d .
H34C H 0.2163 2.0417 0.4454 0.076 Uiso 1 1 calc .
H34D H 0.2584 2.1377 0.4095 0.076 Uiso 1 1 calc .
Cl1 Cl 0.8900(2) 0.0487(2) 0.0204(3) 0.0644(9) Uani 1 1 d .
O101 O 0.8112(9) 0.0189(11) -0.0385(17) 0.158(8) Uani 1 1 d .
O102 O 0.9182(14) 0.1337(8) 0.0479(14) 0.150(7) Uani 1 1 d .
O103 O 0.9446(10) 0.0431(11) -0.0483(8) 0.110(5) Uani 1 1 d .
O104 O 0.8848(9) -0.0031(8) 0.1060(9) 0.099(4) Uani 1 1 d .
Cl2 Cl 0.5340(2) 1.2888(2) 0.3247(2) 0.0644(8) Uani 1 1 d .
O201 O 0.5748(11) 1.3355(12) 0.2362(10) 0.139(6) Uani 1 1 d .
O202 O 0.5867(9) 1.3205(13) 0.4107(8) 0.128(6) Uani 1 1 d .
O203 O 0.492(2) 1.2087(10) 0.3244(17) 0.273(19) Uani 1 1 d .
O204 O 0.4708(11) 1.3133(17) 0.3302(13) 0.169(8) Uani 1 1 d .
O3W O 0.1364(18) 0.7633(19) 0.049(2) 0.209(10) Uani 1 1 d .
O4W O 0.578(3) 1.687(2) 0.757(3) 0.37(3) Uani 1 1 d .
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'
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
N21B Cu1 N11A 88.6(4) 1_655 .
N21B Cu1 N11B 176.4(4) 1_655 .
N11A Cu1 N11B 88.1(3) . .
N21B Cu1 N21A 91.3(3) 1_655 1_565
N11A Cu1 N21A 177.7(4) . 1_565
N11B Cu1 N21A 92.0(3) . 1_565
N21B Cu1 O2W 93.5(3) 1_655 .
N11A Cu1 O2W 89.8(4) . .
N11B Cu1 O2W 87.8(3) . .
N21A Cu1 O2W 92.5(3) 1_565 .
C14A N11A C13A 119.4(10) . .
C14A N11A Cu1 121.0(9) . .
C13A N11A Cu1 118.8(7) . .
C15A C11A C12A 116.9(9) . .
C15A C11A C16A 125.7(12) . .
C12A C11A C16A 117.4(11) . .
C13A C12A C11A 119.1(11) . .
C12A C13A N11A 123.0(10) . .
N11A C14A C15A 117.4(11) . .
C11A C15A C14A 123.7(10) . .
O16A C16A N31A 126.9(12) . .
O16A C16A C11A 116.7(12) . .
N31A C16A C11A 116.5(12) . .
C24A N21A C23A 117.7(9) . .
C24A N21A Cu1 119.6(7) . 1_545
C23A N21A Cu1 122.5(6) . 1_545
C22A C21A C25A 119.3(10) . .
C22A C21A C26A 119.6(11) . .
C25A C21A C26A 121.1(12) . .
C23A C22A C21A 121.0(9) . .
C22A C23A N21A 122.2(9) . .
N21A C24A C25A 120.8(10) . .
C21A C25A C24A 118.8(11) . .
O26A C26A N32A 124.6(11) . .
O26A C26A C21A 121.2(11) . .
N32A C26A C21A 114.3(11) . .
C16A N31A C31A 119.1(12) . .
C26A N32A C34A 122.3(11) . .
N31A C31A C32A 107.4(11) . .
C33A C32A C31A 115.4(13) . .
C32A C33A C34A 113.9(12) . .
N32A C34A C33A 111.2(12) . .
C14B N11B C13B 117.7(10) . .
C14B N11B Cu1 123.8(7) . .
C13B N11B Cu1 118.4(8) . .
C12B C11B C15B 115.9(10) . .
C12B C11B C16B 115.6(11) . .
C15B C11B C16B 128.5(12) . .
C13B C12B C11B 120.4(11) . .
C12B C13B N11B 121.2(12) . .
N11B C14B C15B 126.9(11) . .
C14B C15B C11B 117.8(11) . .
O16B C16B N31B 123.8(11) . .
O16B C16B C11B 121.2(13) . .
N31B C16B C11B 115.0(11) . .
C24B N21B C23B 115.3(9) . .
C24B N21B Cu1 124.7(7) . 1_455
C23B N21B Cu1 119.9(7) . 1_455
C25B C21B C22B 116.2(10) . .
C25B C21B C26B 119.1(10) . .
C22B C21B C26B 124.4(10) . .
C23B C22B C21B 121.7(11) . .
C22B C23B N21B 122.9(10) . .
C25B C24B N21B 123.1(10) . .
C24B C25B C21B 120.7(11) . .
O26B C26B N32B 125.4(10) . .
O26B C26B C21B 118.8(11) . .
N32B C26B C21B 115.8(10) . .
C16B N31B C31B 121.6(11) . .
C26B N32B C34B 120.7(10) . .
N31B C31B C32B 110.6(12) . .
C31B C32B C33B 117.3(14) . .
C34B C33B C32B 117.0(17) . .
N32B C34B C33B 112.3(11) . .
O103 Cl1 O102 111.7(12) . .
O103 Cl1 O104 107.0(7) . .
O102 Cl1 O104 111.8(10) . .
O103 Cl1 O101 102.3(11) . .
O102 Cl1 O101 107.2(11) . .
O104 Cl1 O101 116.5(10) . .
O203 Cl2 O204 104(2) . .
O203 Cl2 O202 111.6(14) . .
O204 Cl2 O202 108.4(10) . .
O203 Cl2 O201 121.2(15) . .
O204 Cl2 O201 96.7(11) . .
O202 Cl2 O201 112.9(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N21B 2.018(8) 1_655
Cu1 N11A 2.035(9) .
Cu1 N11B 2.050(8) .
Cu1 N21A 2.051(8) 1_565
Cu1 O2W 2.380(8) .
N11A C14A 1.340(14) .
N11A C13A 1.404(15) .
O16A C16A 1.313(17) .
C11A C15A 1.336(18) .
C11A C12A 1.437(17) .
C11A C16A 1.509(15) .
C12A C13A 1.347(16) .
C14A C15A 1.449(15) .
C16A N31A 1.297(17) .
N21A C24A 1.345(13) .
N21A C23A 1.363(13) .
N21A Cu1 2.051(8) 1_545
O26A C26A 1.173(15) .
C21A C22A 1.335(17) .
C21A C25A 1.374(16) .
C21A C26A 1.560(15) .
C22A C23A 1.326(14) .
C24A C25A 1.389(15) .
C26A N32A 1.365(16) .
N31A C31A 1.524(16) .
N32A C34A 1.441(16) .
C31A C32A 1.63(2) .
C32A C33A 1.39(2) .
C33A C34A 1.50(2) .
N11B C14B 1.231(13) .
N11B C13B 1.358(15) .
O16B C16B 1.194(15) .
C11B C12B 1.366(18) .
C11B C15B 1.411(17) .
C11B C16B 1.477(16) .
C12B C13B 1.365(16) .
C14B C15B 1.348(16) .
C16B N31B 1.375(18) .
N21B C24B 1.374(14) .
N21B C23B 1.372(13) .
N21B Cu1 2.018(8) 1_455
O26B C26B 1.228(15) .
C21B C25B 1.374(16) .
C21B C22B 1.396(16) .
C21B C26B 1.539(14) .
C22B C23B 1.340(16) .
C24B C25B 1.367(18) .
C26B N32B 1.346(16) .
N31B C31B 1.455(15) .
N32B C34B 1.486(16) .
C31B C32B 1.45(2) .
C32B C33B 1.55(3) .
C33B C34B 1.49(2) .
Cl1 O103 1.378(10) .
Cl1 O102 1.394(11) .
Cl1 O104 1.439(12) .
Cl1 O101 1.463(13) .
Cl2 O203 1.246(17) .
Cl2 O204 1.41(2) .
Cl2 O202 1.407(12) .
Cl2 O201 1.414(14) .
