#------------------------------------------------------------------------------
#$Date: 2017-07-11 15:10:40 +0300 (Tue, 11 Jul 2017) $
#$Revision: 198633 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/50/96/4509692.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4509692
loop_
_publ_author_name
'Li, Lili'
'Liu, Bin'
'Xue, Ganglin'
'Hu, Huaiming'
'Fu, Feng'
'Wang, Jiwu'
_publ_section_title
;
 Three Hybrid Organic−Inorganic Assemblies Based on Different
 Arsenatomolybdates and CuII−Organic Units
;
_journal_issue                   12
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              5206
_journal_paper_doi               10.1021/cg9006718
_journal_volume                  9
_journal_year                    2009
_chemical_formula_sum            'C72 H108 As18 Cu9 Mo18 N48 O96'
_chemical_formula_weight         6829.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           147
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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            1
_cell_length_a                   22.7883(16)
_cell_length_b                   22.7883(16)
_cell_length_c                   9.3807(14)
_cell_measurement_temperature    293(2)
_cell_volume                     4218.8(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0574
_diffrn_reflns_av_sigmaI/netI    0.0567
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            20751
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    6.010
_exptl_absorpt_correction_T_max  0.548
_exptl_absorpt_correction_T_min  0.398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.688
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3255
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.491
_refine_diff_density_min         -1.093
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       0.00002(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         4889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0478P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0928
_reflns_number_gt                3237
_reflns_number_total             4889
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg9006718sup2.cif
_cod_data_source_block           xb2311m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'constrn' was replaced with the
value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_sg_symbol_H-M      p-3
_cod_database_code               4509692
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
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
Mo1 Mo 0.12600(3) 0.16364(3) 0.99870(6) 0.02222(16) Uani 1 1 d .
Mo2 Mo 0.41900(3) 0.58283(3) 0.41955(6) 0.01979(16) Uani 1 1 d .
Mo3 Mo 0.50319(3) 0.75211(3) 0.42591(6) 0.01856(15) Uani 1 1 d .
Cu1 Cu 0.0000 0.0000 1.0000 0.0199(4) Uani 1 6 d S
Cu2 Cu 0.3333 0.6667 0.42133(14) 0.0167(3) Uani 1 3 d S
Cu3 Cu 0.64961(4) 0.85942(4) 0.71954(9) 0.0293(2) Uani 1 1 d .
As1 As 0.03387(4) 0.09377(4) 0.69146(8) 0.0371(2) Uani 1 1 d .
As2 As 0.41700(4) 0.66917(4) 0.11102(8) 0.0329(2) Uani 1 1 d .
As3 As 0.41464(4) 0.75018(4) 0.73246(8) 0.0309(2) Uani 1 1 d .
O1 O 0.0298(2) 0.0877(2) 0.8827(5) 0.0279(11) Uani 1 1 d .
O2 O -0.0497(3) 0.0288(2) 0.6545(5) 0.0388(13) Uani 1 1 d .
O3 O 0.0505(2) 0.1658(2) 1.0888(5) 0.0261(11) Uani 1 1 d .
O4 O 0.1493(2) 0.2245(2) 0.8703(5) 0.0392(13) Uani 1 1 d .
O5 O 0.1790(2) 0.2027(2) 1.1391(5) 0.0394(13) Uani 1 1 d .
O6 O 0.4117(2) 0.6687(2) 0.3033(5) 0.0240(10) Uani 1 1 d .
O7 O 0.4096(2) 0.7447(2) 0.5385(5) 0.0235(10) Uani 1 1 d .
O8 O 0.3313(2) 0.7348(2) 0.7708(5) 0.0338(12) Uani 1 1 d .
O9 O 0.3362(2) 0.5996(2) 0.0750(5) 0.0354(12) Uani 1 1 d .
O10 O 0.3331(2) 0.5216(2) 0.3315(4) 0.0204(10) Uani 1 1 d .
O11 O 0.4683(2) 0.5818(2) 0.2830(5) 0.0331(12) Uani 1 1 d .
O12 O 0.4242(2) 0.5329(2) 0.5485(5) 0.0382(13) Uani 1 1 d .
O13 O 0.4785(2) 0.6670(2) 0.5121(4) 0.0234(10) Uani 1 1 d .
O14 O 0.5581(2) 0.7569(2) 0.2953(5) 0.0321(12) Uani 1 1 d .
O15 O 0.5530(2) 0.8024(2) 0.5624(5) 0.0293(11) Uani 1 1 d .
O16 O 0.5082(3) 0.5284(3) 0.7579(7) 0.0581(16) Uani 1 1 d .
C1 C 0.7212(4) 0.8797(4) 0.4396(9) 0.045(2) Uani 1 1 d .
H1 H 0.7027 0.9046 0.4017 0.054 Uiso 1 1 calc R
C2 C 0.7806(4) 0.8296(4) 0.4568(10) 0.049(2) Uani 1 1 d .
H2 H 0.8099 0.8135 0.4366 0.059 Uiso 1 1 calc R
C3 C 0.7444(4) 0.8194(4) 0.5763(9) 0.043(2) Uani 1 1 d .
H3 H 0.7445 0.7943 0.6542 0.051 Uiso 1 1 calc R
C4 C 0.5827(4) 0.7121(4) 0.7764(8) 0.0383(19) Uani 1 1 d .
H4 H 0.5482 0.7039 0.7126 0.046 Uiso 1 1 calc R
C5 C 0.6463(4) 0.6964(4) 0.9265(10) 0.055(2) Uani 1 1 d .
H5 H 0.6642 0.6764 0.9853 0.066 Uiso 1 1 calc R
C6 C 0.6711(4) 0.7618(4) 0.9030(8) 0.041(2) Uani 1 1 d .
H6 H 0.7103 0.7962 0.9449 0.050 Uiso 1 1 calc R
C7 C 0.7027(4) 1.0058(4) 0.7126(9) 0.043(2) Uani 1 1 d .
H7 H 0.7299 1.0116 0.7914 0.051 Uiso 1 1 calc R
C8 C 0.6508(5) 1.0277(4) 0.5443(10) 0.056(2) Uani 1 1 d .
H8 H 0.6357 1.0499 0.4842 0.067 Uiso 1 1 calc R
C9 C 0.6345(4) 0.9622(4) 0.5393(9) 0.044(2) Uani 1 1 d .
H9 H 0.6045 0.9306 0.4743 0.052 Uiso 1 1 calc R
C10 C 0.5830(4) 0.8463(4) 1.0046(9) 0.044(2) Uani 1 1 d .
H10 H 0.5998 0.8198 1.0419 0.053 Uiso 1 1 calc R
C11 C 0.5276(4) 0.9003(4) 0.9883(9) 0.042(2) Uani 1 1 d .
H11 H 0.5002 0.9186 1.0090 0.051 Uiso 1 1 calc R
C12 C 0.5606(4) 0.9057(4) 0.8657(8) 0.0379(19) Uani 1 1 d .
H12 H 0.5594 0.9290 0.7855 0.045 Uiso 1 1 calc R
N1 N 0.7069(3) 0.8517(3) 0.5664(6) 0.0336(15) Uani 1 1 d .
N2 N 0.7656(3) 0.8679(3) 0.3724(7) 0.0455(18) Uani 1 1 d .
H2A H 0.7820 0.8824 0.2888 0.055 Uiso 1 1 calc R
N3 N 0.6317(3) 0.7721(3) 0.8094(6) 0.0291(14) Uani 1 1 d .
N4 N 0.5880(3) 0.6642(3) 0.8449(7) 0.0446(17) Uani 1 1 d .
H4A H 0.5604 0.6212 0.8396 0.054 Uiso 1 1 calc R
N5 N 0.6681(3) 0.9487(3) 0.6435(6) 0.0334(15) Uani 1 1 d .
N6 N 0.6942(4) 1.0545(3) 0.6562(9) 0.055(2) Uani 1 1 d .
H6A H 0.7128 1.0957 0.6853 0.067 Uiso 1 1 calc R
N7 N 0.5964(3) 0.8720(3) 0.8750(6) 0.0334(15) Uani 1 1 d .
N8 N 0.5432(3) 0.8622(3) 1.0753(7) 0.0451(17) Uani 1 1 d .
H8A H 0.5294 0.8507 1.1615 0.054 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 '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'
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
O5 Mo1 O4 105.6(2) . .
O5 Mo1 O3 102.4(2) . 5_557
O4 Mo1 O3 96.9(2) . 5_557
O5 Mo1 O3 93.2(2) . .
O4 Mo1 O3 101.9(2) . .
O3 Mo1 O3 151.4(2) 5_557 .
O5 Mo1 O1 157.8(2) . .
O4 Mo1 O1 94.0(2) . .
O3 Mo1 O1 84.97(17) 5_557 .
O3 Mo1 O1 72.45(17) . .
O5 Mo1 O1 88.4(2) . 5_557
O4 Mo1 O1 162.9(2) . 5_557
O3 Mo1 O1 70.19(16) 5_557 5_557
O3 Mo1 O1 86.66(17) . 5_557
O1 Mo1 O1 74.3(2) . 5_557
O12 Mo2 O11 104.9(2) . .
O12 Mo2 O13 95.5(2) . .
O11 Mo2 O13 102.22(19) . .
O12 Mo2 O10 101.8(2) . .
O11 Mo2 O10 96.04(19) . .
O13 Mo2 O10 150.64(17) . .
O12 Mo2 O7 92.5(2) . 3_565
O11 Mo2 O7 160.5(2) . 3_565
O13 Mo2 O7 84.49(16) . 3_565
O10 Mo2 O7 71.35(16) . 3_565
O12 Mo2 O6 162.8(2) . .
O11 Mo2 O6 89.06(19) . .
O13 Mo2 O6 71.41(16) . .
O10 Mo2 O6 86.25(16) . .
O7 Mo2 O6 75.59(15) 3_565 .
O15 Mo3 O14 105.8(2) . .
O15 Mo3 O13 97.06(19) . .
O14 Mo3 O13 101.7(2) . .
O15 Mo3 O10 101.71(19) . 2_665
O14 Mo3 O10 95.03(19) . 2_665
O13 Mo3 O10 150.39(17) . 2_665
O15 Mo3 O6 161.23(19) . .
O14 Mo3 O6 91.50(19) . .
O13 Mo3 O6 71.81(16) . .
O10 Mo3 O6 83.58(16) 2_665 .
O15 Mo3 O7 89.23(19) . .
O14 Mo3 O7 161.63(19) . .
O13 Mo3 O7 86.53(16) . .
O10 Mo3 O7 71.15(16) 2_665 .
O6 Mo3 O7 75.32(15) . .
O1 Cu1 O1 180.0(2) 2 5_557
O1 Cu1 O1 94.51(17) 2 3
O1 Cu1 O1 85.49(17) 5_557 3
O1 Cu1 O1 85.49(17) 2 4_557
O1 Cu1 O1 94.51(17) 5_557 4_557
O1 Cu1 O1 85.49(17) 3 4_557
O1 Cu1 O1 94.51(17) 2 .
O1 Cu1 O1 85.49(17) 5_557 .
O1 Cu1 O1 94.51(17) 3 .
O1 Cu1 O1 180.00(15) 4_557 .
O1 Cu1 O1 85.49(17) 2 6_557
O1 Cu1 O1 94.51(17) 5_557 6_557
O1 Cu1 O1 180.000(1) 3 6_557
O1 Cu1 O1 94.51(17) 4_557 6_557
O1 Cu1 O1 85.49(17) . 6_557
O7 Cu2 O7 94.53(17) 2_665 .
O7 Cu2 O7 94.53(17) 2_665 3_565
O7 Cu2 O7 94.53(17) . 3_565
O7 Cu2 O6 85.43(16) 2_665 2_665
O7 Cu2 O6 85.70(16) . 2_665
O7 Cu2 O6 179.77(19) 3_565 2_665
O7 Cu2 O6 85.70(16) 2_665 3_565
O7 Cu2 O6 179.77(17) . 3_565
O7 Cu2 O6 85.43(16) 3_565 3_565
O6 Cu2 O6 94.34(17) 2_665 3_565
O7 Cu2 O6 179.77(17) 2_665 .
O7 Cu2 O6 85.43(16) . .
O7 Cu2 O6 85.70(16) 3_565 .
O6 Cu2 O6 94.34(17) 2_665 .
O6 Cu2 O6 94.34(17) 3_565 .
N5 Cu3 N7 87.1(2) . .
N5 Cu3 N3 176.1(2) . .
N7 Cu3 N3 89.9(2) . .
N5 Cu3 N1 91.1(2) . .
N7 Cu3 N1 177.0(2) . .
N3 Cu3 N1 91.9(2) . .
N5 Cu3 O15 90.1(2) . .
N7 Cu3 O15 93.9(2) . .
N3 Cu3 O15 92.5(2) . .
N1 Cu3 O15 88.5(2) . .
O2 As1 O2 99.7(3) . 3
O2 As1 O1 98.0(2) . .
O2 As1 O1 100.0(2) 3 .
O9 As2 O9 99.3(3) . 2_665
O9 As2 O6 98.6(2) . .
O9 As2 O6 98.7(2) 2_665 .
O8 As3 O8 99.8(3) 3_565 .
O8 As3 O7 99.1(2) 3_565 .
O8 As3 O7 99.4(2) . .
As1 O1 Cu1 125.6(2) . .
As1 O1 Mo1 115.1(2) . .
Cu1 O1 Mo1 101.83(18) . .
As1 O1 Mo1 117.1(2) . 6_557
Cu1 O1 Mo1 98.31(18) . 6_557
Mo1 O1 Mo1 92.91(15) . 6_557
As1 O2 As1 132.2(3) . 2
Mo1 O3 Mo1 122.1(2) 6_557 .
As2 O6 Cu2 125.8(2) . .
As2 O6 Mo3 117.6(2) . .
Cu2 O6 Mo3 99.49(17) . .
As2 O6 Mo2 116.2(2) . .
Cu2 O6 Mo2 98.84(17) . .
Mo3 O6 Mo2 92.53(15) . .
As3 O7 Cu2 125.8(2) . .
As3 O7 Mo2 116.7(2) . 2_665
Cu2 O7 Mo2 99.86(18) . 2_665
As3 O7 Mo3 115.3(2) . .
Cu2 O7 Mo3 99.69(17) . .
Mo2 O7 Mo3 93.69(15) 2_665 .
As3 O8 As3 131.6(3) 2_665 .
As2 O9 As2 132.9(3) . 3_565
Mo3 O10 Mo2 121.1(2) 3_565 .
Mo3 O13 Mo2 121.8(2) . .
Mo3 O15 Cu3 159.3(3) . .
N1 C1 N2 111.2(7) . .
C3 C2 N2 105.8(7) . .
C2 C3 N1 110.0(7) . .
N3 C4 N4 111.6(7) . .
C6 C5 N4 105.2(7) . .
C5 C6 N3 110.8(7) . .
N5 C7 N6 111.5(8) . .
C9 C8 N6 105.1(8) . .
C8 C9 N5 110.3(8) . .
N8 C10 N7 112.4(7) . .
C12 C11 N8 105.0(7) . .
C11 C12 N7 110.8(7) . .
C1 N1 C3 104.5(6) . .
C1 N1 Cu3 128.4(5) . .
C3 N1 Cu3 127.0(5) . .
C1 N2 C2 108.5(7) . .
C4 N3 C6 105.6(6) . .
C4 N3 Cu3 125.8(5) . .
C6 N3 Cu3 128.2(5) . .
C4 N4 C5 106.8(6) . .
C7 N5 C9 105.0(7) . .
C7 N5 Cu3 123.6(5) . .
C9 N5 Cu3 128.9(5) . .
C7 N6 C8 108.1(7) . .
C10 N7 C12 103.7(6) . .
C10 N7 Cu3 129.0(5) . .
C12 N7 Cu3 127.1(5) . .
C10 N8 C11 108.1(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O5 1.706(5) .
Mo1 O4 1.709(5) .
Mo1 O3 1.926(4) 5_557
Mo1 O3 1.940(4) .
Mo1 O1 2.279(4) .
Mo1 O1 2.387(4) 5_557
Mo2 O12 1.704(5) .
Mo2 O11 1.711(4) .
Mo2 O13 1.916(4) .
Mo2 O10 1.931(4) .
Mo2 O7 2.294(4) 3_565
Mo2 O6 2.318(4) .
Mo3 O15 1.714(4) .
Mo3 O14 1.715(4) .
Mo3 O13 1.908(4) .
Mo3 O10 1.924(4) 2_665
Mo3 O6 2.306(4) .
Mo3 O7 2.308(4) .
Cu1 O1 2.076(4) 2
Cu1 O1 2.076(4) 5_557
Cu1 O1 2.076(4) 3
Cu1 O1 2.076(4) 4_557
Cu1 O1 2.076(4) .
Cu1 O1 2.076(4) 6_557
Cu2 O7 2.074(4) 2_665
Cu2 O7 2.074(4) .
Cu2 O7 2.074(4) 3_565
Cu2 O6 2.082(4) 2_665
Cu2 O6 2.082(4) 3_565
Cu2 O6 2.082(4) .
Cu3 N5 1.993(6) .
Cu3 N7 2.007(6) .
Cu3 N3 2.007(5) .
Cu3 N1 2.007(6) .
Cu3 O15 2.418(4) .
As1 O2 1.766(5) .
As1 O2 1.784(5) 3
As1 O1 1.798(5) .
As2 O9 1.761(5) .
As2 O9 1.788(5) 2_665
As2 O6 1.807(4) .
As3 O8 1.781(5) 3_565
As3 O8 1.786(5) .
As3 O7 1.824(5) .
O1 Mo1 2.387(4) 6_557
O2 As1 1.784(5) 2
O3 Mo1 1.926(4) 6_557
O7 Mo2 2.294(4) 2_665
O8 As3 1.781(5) 2_665
O9 As2 1.788(5) 3_565
O10 Mo3 1.924(4) 3_565
C1 N1 1.311(9) .
C1 N2 1.328(9) .
C2 C3 1.340(11) .
C2 N2 1.342(10) .
C3 N1 1.382(9) .
C4 N3 1.297(9) .
C4 N4 1.323(8) .
C5 C6 1.322(10) .
C5 N4 1.385(10) .
C6 N3 1.358(8) .
C7 N5 1.307(9) .
C7 N6 1.328(10) .
C8 C9 1.347(11) .
C8 N6 1.358(11) .
C9 N5 1.368(9) .
C10 N8 1.313(9) .
C10 N7 1.317(9) .
C11 C12 1.345(10) .
C11 N8 1.360(10) .
C12 N7 1.373(9) .
