#------------------------------------------------------------------------------
#$Date: 2019-11-08 01:35:50 +0100 (vie 08 de nov de 2019) $
#$Revision: 224807 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/82/7058257.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_7058257
loop_
_publ_author_name
'Ying, Jun'
'Chen, Ya-Guang'
'Wang, Xiu-Yan'
_publ_section_title
;
 Two isopolytungstate compounds based on rare [W6O22]8− and
 [H2W12O42]10− fragments captured by premade copper(ii) complexes
;
_journal_issue                   17
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              6765
_journal_paper_doi               10.1039/C8NJ06367B
_journal_volume                  43
_journal_year                    2019
_chemical_formula_sum            'C40 H44 Cu4 N8 O28 W6'
_chemical_formula_weight         2442
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-12-02 deposited with the CCDC.    2019-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                102.389(3)
_cell_angle_beta                 106.937(3)
_cell_angle_gamma                109.667(2)
_cell_formula_units_Z            1
_cell_length_a                   9.2019(16)
_cell_length_b                   12.776(2)
_cell_length_c                   13.891(2)
_cell_measurement_reflns_used    7371
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1.80
_cell_volume                     1379.7(4)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7371
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    14.051
_exptl_absorpt_correction_T_max  0.245
_exptl_absorpt_correction_T_min  0.202
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.925
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.060
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         4829
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0322
_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)+(0.0189P)²+5.6611P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0565
_refine_ls_wR_factor_ref         0.0600
_reflns_number_gt                3966
_reflns_number_total             4853
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8nj06367b2.cif
_cod_data_source_block           compound-1
_cod_depositor_comments
'Adding full bibliography for 7058257--7058258.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7058257
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
W1 W 0.41070(4) 0.36575(3) 0.01461(3) 0.01501(9) Uani 1 1 d .
W2 W 0.79127(4) 0.56135(3) 0.18449(3) 0.01764(9) Uani 1 1 d .
W3 W 0.45236(5) 0.30635(3) -0.21917(3) 0.01968(10) Uani 1 1 d .
O1 O 0.2178(7) 0.3777(5) -0.0514(4) 0.0190(13) Uani 1 1 d .
O1W O 1.0118(8) 0.4067(6) 0.0614(5) 0.0316(16) Uani 1 1 d .
O2 O 0.5276(7) 0.5350(5) 0.1014(4) 0.0159(12) Uani 1 1 d .
O2W O 0.3714(14) -0.0165(8) -0.4601(9) 0.111(4) Uani 1 1 d .
O3 O 0.3836(9) 0.1661(5) -0.3105(5) 0.0331(16) Uani 1 1 d .
O3W O 1.0194(12) 0.8919(9) 0.4577(8) 0.096(3) Uani 1 1 d .
O4 O 0.9974(8) 0.5880(5) 0.2150(5) 0.0294(15) Uani 1 1 d .
O5 O 0.7451(7) 0.4967(5) 0.2825(5) 0.0245(14) Uani 1 1 d .
O6 O 0.3678(8) 0.3003(5) 0.1054(5) 0.0246(14) Uani 1 1 d .
O7 O 0.6647(8) 0.3418(5) -0.1395(5) 0.0256(15) Uani 1 1 d .
O8 O 0.7899(7) 0.7038(5) 0.2507(4) 0.0237(14) Uani 1 1 d .
O9 O 0.3944(7) 0.2499(5) -0.0977(5) 0.0210(13) Uani 1 1 d .
O10 O 0.6661(7) 0.4051(4) 0.0680(4) 0.0152(12) Uani 1 1 d .
O11 O 0.4804(7) 0.3992(5) -0.2993(5) 0.0241(14) Uani 1 1 d .
Cu1 Cu 0.56117(14) 0.47175(10) 0.32549(9) 0.0232(3) Uani 1 1 d .
Cu2 Cu 0.73078(14) 0.29604(9) -0.01255(9) 0.0217(2) Uani 1 1 d .
C1 C 0.8165(13) 0.1665(10) -0.1751(9) 0.042(3) Uani 1 1 d .
H1A H 0.8175 0.2264 -0.2034 0.051 Uiso 1 1 calc R
C2 C 0.8558(15) 0.0780(10) -0.2232(10) 0.054(3) Uani 1 1 d .
H2A H 0.8842 0.0791 -0.2820 0.065 Uiso 1 1 calc R
C3 C 0.8517(15) -0.0112(10) -0.1813(10) 0.054(3) Uani 1 1 d .
H3A H 0.8758 -0.0721 -0.2120 0.064 Uiso 1 1 calc R
C4 C 0.8113(13) -0.0080(9) -0.0938(8) 0.036(3) Uani 1 1 d .
H4B H 0.8077 -0.0673 -0.0645 0.043 Uiso 1 1 calc R
C5 C 0.7763(12) 0.0817(8) -0.0490(7) 0.028(2) Uani 1 1 d .
C6 C 0.7296(12) 0.0920(7) 0.0449(7) 0.026(2) Uani 1 1 d .
C7 C 0.7130(13) 0.0121(8) 0.0975(8) 0.039(3) Uani 1 1 d .
H7A H 0.7330 -0.0539 0.0753 0.046 Uiso 1 1 calc R
C8 C 0.6663(13) 0.0298(9) 0.1843(9) 0.042(3) Uani 1 1 d .
H8A H 0.6563 -0.0230 0.2215 0.051 Uiso 1 1 calc R
C9 C 0.6356(13) 0.1266(9) 0.2132(8) 0.037(3) Uani 1 1 d .
H9A H 0.6008 0.1394 0.2694 0.044 Uiso 1 1 calc R
C10 C 0.6563(11) 0.2057(8) 0.1590(8) 0.027(2) Uani 1 1 d .
H10A H 0.6371 0.2722 0.1804 0.033 Uiso 1 1 calc R
C11 C 0.7858(12) 0.3868(8) 0.4548(7) 0.029(2) Uani 1 1 d .
H11A H 0.8656 0.4268 0.4313 0.035 Uiso 1 1 calc R
C12 C 0.8299(13) 0.3335(9) 0.5285(8) 0.034(2) Uani 1 1 d .
H12A H 0.9378 0.3378 0.5544 0.041 Uiso 1 1 calc R
C13 C 0.7133(14) 0.2752(8) 0.5620(7) 0.035(3) Uani 1 1 d .
H13A H 0.7422 0.2409 0.6129 0.042 Uiso 1 1 calc R
C14 C 0.5525(14) 0.2660(8) 0.5218(8) 0.033(2) Uani 1 1 d .
H14A H 0.4702 0.2223 0.5417 0.040 Uiso 1 1 calc R
C15 C 0.5164(12) 0.3248(7) 0.4496(7) 0.024(2) Uani 1 1 d .
C16 C 0.3524(11) 0.3302(7) 0.4073(7) 0.024(2) Uani 1 1 d .
C17 C 0.2103(14) 0.2705(9) 0.4213(8) 0.038(3) Uani 1 1 d .
H17A H 0.2106 0.2208 0.4614 0.046 Uiso 1 1 calc R
C18 C 0.0661(13) 0.2843(10) 0.3755(9) 0.049(3) Uani 1 1 d .
H18A H -0.0314 0.2431 0.3839 0.058 Uiso 1 1 calc R
C19 C 0.0670(13) 0.3581(10) 0.3183(8) 0.043(3) Uani 1 1 d .
H19A H -0.0291 0.3683 0.2874 0.052 Uiso 1 1 calc R
C20 C 0.2153(12) 0.4185(9) 0.3066(8) 0.032(2) Uani 1 1 d .
H20A H 0.2182 0.4712 0.2695 0.038 Uiso 1 1 calc R
N1 N 0.7778(10) 0.1678(6) -0.0908(6) 0.0274(18) Uani 1 1 d .
N2 N 0.7035(9) 0.1893(6) 0.0766(6) 0.0227(17) Uani 1 1 d .
N3 N 0.6306(9) 0.3824(6) 0.4161(6) 0.0225(17) Uani 1 1 d .
N4 N 0.3526(10) 0.4019(7) 0.3478(6) 0.0274(18) 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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
O6 W1 O1 103.3(2) . .
O6 W1 O9 106.8(2) . .
O1 W1 O9 98.5(2) . .
O6 W1 O2 102.8(2) . .
O1 W1 O2 92.4(2) . .
O9 W1 O2 145.0(2) . .
O6 W1 O10 97.5(2) . .
O1 W1 O10 157.6(2) . .
O9 W1 O10 83.3(2) . .
O2 W1 O10 74.7(2) . .
O6 W1 O2 176.7(2) . 2_665
O1 W1 O2 76.2(2) . 2_665
O9 W1 O2 76.5(2) . 2_665
O2 W1 O2 74.0(2) . 2_665
O10 W1 O2 82.56(19) . 2_665
O4 W2 O5 102.2(3) . .
O4 W2 O8 106.7(3) . .
O5 W2 O8 94.1(2) . .
O4 W2 O10 103.8(3) . .
O5 W2 O10 91.9(2) . .
O8 W2 O10 146.9(2) . .
O4 W2 O1 91.1(2) . 2_665
O5 W2 O1 166.4(2) . 2_665
O8 W2 O1 84.9(2) . 2_665
O10 W2 O1 81.9(2) . 2_665
O4 W2 O2 163.4(2) . .
O5 W2 O2 93.8(2) . .
O8 W2 O2 76.0(2) . .
O10 W2 O2 71.1(2) . .
O1 W2 O2 72.67(19) 2_665 .
O3 W3 O7 103.1(3) . .
O3 W3 O11 102.6(3) . .
O7 W3 O11 101.4(3) . .
O3 W3 O8 94.4(3) . 2_665
O7 W3 O8 156.8(2) . 2_665
O11 W3 O8 89.2(2) . 2_665
O3 W3 O9 96.6(2) . .
O7 W3 O9 85.8(2) . .
O11 W3 O9 157.2(2) . .
O8 W3 O9 77.1(2) 2_665 .
O3 W3 O2 164.6(3) . 2_665
O7 W3 O2 88.6(2) . 2_665
O11 W3 O2 84.5(2) . 2_665
O8 W3 O2 71.8(2) 2_665 2_665
O9 W3 O2 74.01(19) . 2_665
W1 O1 W2 115.3(2) . 2_665
W1 O2 W3 151.0(3) . 2_665
W1 O2 W2 103.3(2) . .
W3 O2 W2 95.7(2) 2_665 .
W1 O2 W1 106.0(2) . 2_665
W3 O2 W1 93.94(18) 2_665 2_665
W2 O2 W1 94.46(18) . 2_665
W2 O5 Cu1 130.0(3) . .
W3 O7 Cu2 123.4(3) . .
W2 O8 W3 113.4(3) . 2_665
W1 O9 W3 115.4(3) . .
Cu2 O10 W2 134.5(3) . .
Cu2 O10 W1 117.0(3) . .
W2 O10 W1 108.2(2) . .
W3 O11 Cu1 141.2(3) . 2_665
O11 Cu1 O5 97.2(2) 2_665 .
O11 Cu1 N3 155.1(3) 2_665 .
O5 Cu1 N3 92.9(3) . .
O11 Cu1 N4 93.8(3) 2_665 .
O5 Cu1 N4 164.8(3) . .
N3 Cu1 N4 81.2(3) . .
O10 Cu2 O7 91.7(2) . .
O10 Cu2 N1 172.7(3) . .
O7 Cu2 N1 92.6(3) . .
O10 Cu2 N2 93.8(2) . .
O7 Cu2 N2 155.4(3) . .
N1 Cu2 N2 79.8(3) . .
O10 Cu2 O1W 98.6(2) . .
O7 Cu2 O1W 101.1(2) . .
N1 Cu2 O1W 86.4(3) . .
N2 Cu2 O1W 101.7(3) . .
N1 C1 C2 121.9(10) . .
N1 C1 H1A 119.0 . .
C2 C1 H1A 119.0 . .
C3 C2 C1 118.5(10) . .
C3 C2 H2A 120.7 . .
C1 C2 H2A 120.7 . .
C4 C3 C2 118.5(10) . .
C4 C3 H3A 120.7 . .
C2 C3 H3A 120.7 . .
C5 C4 C3 120.5(9) . .
C5 C4 H4B 119.8 . .
C3 C4 H4B 119.8 . .
N1 C5 C4 121.1(8) . .
N1 C5 C6 114.6(7) . .
C4 C5 C6 124.3(8) . .
N2 C6 C7 121.1(9) . .
N2 C6 C5 114.1(7) . .
C7 C6 C5 124.8(8) . .
C6 C7 C8 120.0(9) . .
C6 C7 H7A 120.0 . .
C8 C7 H7A 120.0 . .
C9 C8 C7 118.1(9) . .
C9 C8 H8A 120.9 . .
C7 C8 H8A 120.9 . .
C8 C9 C10 119.9(9) . .
C8 C9 H9A 120.0 . .
C10 C9 H9A 120.0 . .
N2 C10 C9 121.8(8) . .
N2 C10 H10A 119.1 . .
C9 C10 H10A 119.1 . .
N3 C11 C12 122.0(8) . .
N3 C11 H11A 119.0 . .
C12 C11 H11A 119.0 . .
C13 C12 C11 118.8(9) . .
C13 C12 H12A 120.6 . .
C11 C12 H12A 120.6 . .
C12 C13 C14 120.8(9) . .
C12 C13 H13A 119.6 . .
C14 C13 H13A 119.6 . .
C13 C14 C15 117.8(9) . .
C13 C14 H14A 121.1 . .
C15 C14 H14A 121.1 . .
N3 C15 C14 121.7(9) . .
N3 C15 C16 115.0(7) . .
C14 C15 C16 123.3(8) . .
N4 C16 C17 120.6(9) . .
N4 C16 C15 112.6(7) . .
C17 C16 C15 126.7(8) . .
C16 C17 C18 119.6(9) . .
C16 C17 H17A 120.2 . .
C18 C17 H17A 120.2 . .
C19 C18 C17 119.9(10) . .
C19 C18 H18A 120.1 . .
C17 C18 H18A 120.1 . .
C18 C19 C20 118.8(10) . .
C18 C19 H19A 120.6 . .
C20 C19 H19A 120.6 . .
N4 C20 C19 121.2(9) . .
N4 C20 H20A 119.4 . .
C19 C20 H20A 119.4 . .
C1 N1 C5 119.5(8) . .
C1 N1 Cu2 124.4(6) . .
C5 N1 Cu2 116.1(6) . .
C10 N2 C6 119.0(7) . .
C10 N2 Cu2 125.5(6) . .
C6 N2 Cu2 115.4(6) . .
C15 N3 C11 118.9(7) . .
C15 N3 Cu1 115.1(6) . .
C11 N3 Cu1 125.6(6) . .
C20 N4 C16 119.8(8) . .
C20 N4 Cu1 124.4(6) . .
C16 N4 Cu1 115.8(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O6 1.722(5) .
W1 O1 1.819(6) .
W1 O9 1.835(5) .
W1 O2 1.961(5) .
W1 O10 2.087(5) .
W1 O2 2.334(5) 2_665
W2 O4 1.711(6) .
W2 O5 1.816(5) .
W2 O8 1.860(6) .
W2 O10 1.978(5) .
W2 O1 2.146(5) 2_665
W2 O2 2.233(5) .
W3 O3 1.736(6) .
W3 O7 1.783(6) .
W3 O11 1.800(5) .
W3 O8 2.095(6) 2_665
W3 O9 2.107(5) .
W3 O2 2.229(5) 2_665
O1 W2 2.146(5) 2_665
O1W Cu2 2.260(6) .
O2 W3 2.229(5) 2_665
O2 W1 2.334(5) 2_665
O5 Cu1 1.905(5) .
O7 Cu2 1.969(5) .
O8 W3 2.095(6) 2_665
O10 Cu2 1.955(5) .
O11 Cu1 1.897(5) 2_665
Cu1 O11 1.897(5) 2_665
Cu1 N3 1.983(7) .
Cu1 N4 1.972(7) .
Cu2 N1 2.010(7) .
Cu2 N2 2.033(7) .
C1 N1 1.318(11) .
C1 C2 1.396(13) .
C1 H1A 0.9300 .
C2 C3 1.380(15) .
C2 H2A 0.9300 .
C3 C4 1.368(14) .
C3 H3A 0.9300 .
C4 C5 1.364(12) .
C4 H4B 0.9300 .
C5 N1 1.346(10) .
C5 C6 1.482(12) .
C6 N2 1.351(10) .
C6 C7 1.371(12) .
C7 C8 1.393(13) .
C7 H7A 0.9300 .
C8 C9 1.364(13) .
C8 H8A 0.9300 .
C9 C10 1.379(11) .
C9 H9A 0.9300 .
C10 N2 1.338(10) .
C10 H10A 0.9300 .
C11 N3 1.348(11) .
C11 C12 1.385(12) .
C11 H11A 0.9300 .
C12 C13 1.352(13) .
C12 H12A 0.9300 .
C13 C14 1.374(13) .
C13 H13A 0.9300 .
C14 C15 1.406(12) .
C14 H14A 0.9300 .
C15 N3 1.333(10) .
C15 C16 1.483(12) .
C16 N4 1.359(10) .
C16 C17 1.367(12) .
C17 C18 1.382(14) .
C17 H17A 0.9300 .
C18 C19 1.356(14) .
C18 H18A 0.9300 .
C19 C20 1.399(13) .
C19 H19A 0.9300 .
C20 N4 1.334(11) .
C20 H20A 0.9300 .
