#------------------------------------------------------------------------------
#$Date: 2025-08-22 10:56:18 +0200 (Fri 22 de Aug de 2025) $
#$Revision: 301860 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/20/7122000.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_7122000
loop_
_publ_author_name
'Faulkner, Robert A.'
'Patmore, Nathan J.'
'Rice, Craig R.'
'Slater, Christopher'
_publ_section_title
;
 Dihydrogen phosphate-containing dinuclear double assemblies that
 demonstrate phosphate reactivity to the tetrafluoroborate anion.
;
_journal_issue                   66
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9159
_journal_page_last               9162
_journal_paper_doi               10.1039/c8cc04900a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_sum            'C40 H32 Cu2 F12 N12 O12 S8'
_chemical_formula_weight         1484.33
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-06-16 deposited with the CCDC.
2018-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                67.525(3)
_cell_angle_beta                 73.066(3)
_cell_angle_gamma                83.669(3)
_cell_formula_units_Z            1
_cell_length_a                   9.7479(10)
_cell_length_b                   10.8987(11)
_cell_length_c                   14.1786(14)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.34
_cell_volume                     1331.6(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.0858
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22989
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.578
_diffrn_reflns_theta_min         2.072
_exptl_absorpt_coefficient_mu    1.227
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_description       block
_exptl_crystal_F_000             746
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.942
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         8122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0504P)²+0.6761P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1288
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5735
_reflns_number_total             8122
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8cc04900a2.cif
_cod_data_source_block           mo_Chris_Ledatrif_5_0m
_cod_depositor_comments
'Adding full bibliography for 7122000--7122004.cif.'
_cod_database_code               7122000
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Cu1 Cu 0.40837(3) 0.71264(3) 0.32144(2) 0.01567(9) Uani 1 1 d . .
S1 S 0.56338(8) 0.44194(7) 0.14098(6) 0.02217(16) Uani 1 1 d . .
S2 S 0.12290(8) 0.28305(7) 0.08184(6) 0.02421(17) Uani 1 1 d . .
S3 S 0.34895(7) 0.37610(6) 0.49236(5) 0.01869(15) Uani 1 1 d . .
S4 S 0.23725(9) 0.90411(7) 0.56424(6) 0.02629(17) Uani 1 1 d . .
F1 F 0.1724(3) 0.3837(3) 0.38404(18) 0.0648(7) Uani 1 1 d . .
F2 F 0.0713(2) 0.39149(19) 0.53850(18) 0.0475(6) Uani 1 1 d . .
F3 F 0.1549(2) 0.20743(18) 0.52363(17) 0.0439(5) Uani 1 1 d . .
F4 F 0.2558(3) 0.1781(3) 0.23012(18) 0.0734(8) Uani 1 1 d . .
F5 F 0.2845(2) 0.07048(19) 0.1266(2) 0.0554(6) Uani 1 1 d . .
F6 F 0.3953(2) 0.25322(19) 0.07345(18) 0.0445(5) Uani 1 1 d . .
N1 N 0.5364(2) 0.8743(2) 0.23677(17) 0.0170(5) Uani 1 1 d . .
N2 N 0.3454(2) 0.8042(2) 0.42145(17) 0.0158(4) Uani 1 1 d . .
N3 N 0.1854(2) 0.6605(2) 0.57239(18) 0.0198(5) Uani 1 1 d . .
H3A H 0.1867 0.6075 0.5384 0.024 Uiso 1 1 calc R U
N4 N 0.2274(2) 0.7462(2) 0.25979(18) 0.0191(5) Uani 1 1 d . .
N5 N 0.4715(2) 0.6148(2) 0.22654(17) 0.0155(4) Uani 1 1 d . .
N6 N 0.6911(2) 0.5163(2) 0.25455(18) 0.0189(5) Uani 1 1 d . .
H6 H 0.6983 0.5649 0.2902 0.023 Uiso 1 1 calc R U
O1 O 0.3498(2) 0.52083(18) 0.44763(15) 0.0271(5) Uani 1 1 d . .
O2 O 0.3346(2) 0.3256(2) 0.60443(16) 0.0295(5) Uani 1 1 d . .
O3 O 0.4517(2) 0.31299(19) 0.43059(16) 0.0269(5) Uani 1 1 d . .
O4 O 0.1327(2) 0.4096(2) 0.08856(18) 0.0317(5) Uani 1 1 d . .
O5 O 0.1607(3) 0.2842(3) -0.02382(19) 0.0446(6) Uani 1 1 d . .
O6 O -0.0008(3) 0.2051(2) 0.1544(2) 0.0489(7) Uani 1 1 d . .
C1 C 0.6343(3) 0.8979(3) 0.1433(2) 0.0233(6) Uani 1 1 d . .
H1 H 0.6459 0.8351 0.1100 0.028 Uiso 1 1 calc R U
C2 C 0.7188(3) 1.0101(3) 0.0934(2) 0.0280(7) Uani 1 1 d . .
H2 H 0.7885 1.0239 0.0275 0.034 Uiso 1 1 calc R U
C3 C 0.7002(3) 1.1026(3) 0.1415(3) 0.0296(7) Uani 1 1 d . .
H3 H 0.7573 1.1808 0.1087 0.035 Uiso 1 1 calc R U
C4 C 0.5990(3) 1.0803(3) 0.2364(2) 0.0251(6) Uani 1 1 d . .
H4 H 0.5847 1.1430 0.2701 0.030 Uiso 1 1 calc R U
C5 C 0.5174(3) 0.9648(2) 0.2831(2) 0.0172(5) Uani 1 1 d . .
C6 C 0.4082(3) 0.9280(2) 0.3850(2) 0.0177(5) Uani 1 1 d . .
C7 C 0.3623(3) 0.9959(3) 0.4506(2) 0.0251(6) Uani 1 1 d . .
H7 H 0.3944 1.0820 0.4362 0.030 Uiso 1 1 calc R U
C8 C 0.2557(3) 0.7751(2) 0.5177(2) 0.0176(5) Uani 1 1 d . .
C9 C 0.1060(3) 0.6156(3) 0.6848(2) 0.0230(6) Uani 1 1 d . .
H9A H 0.0491 0.5362 0.7022 0.028 Uiso 1 1 calc R U
H9B H 0.0379 0.6861 0.6965 0.028 Uiso 1 1 calc R U
C10 C 0.1150(3) 0.8256(3) 0.2735(2) 0.0235(6) Uani 1 1 d . .
H10 H 0.1091 0.8725 0.3189 0.028 Uiso 1 1 calc R U
C11 C 0.0071(3) 0.8423(3) 0.2247(3) 0.0313(7) Uani 1 1 d . .
H11 H -0.0707 0.9009 0.2350 0.038 Uiso 1 1 calc R U
C12 C 0.0149(3) 0.7717(3) 0.1601(3) 0.0301(7) Uani 1 1 d . .
H12 H -0.0592 0.7795 0.1270 0.036 Uiso 1 1 calc R U
C13 C 0.1311(3) 0.6898(3) 0.1442(2) 0.0230(6) Uani 1 1 d . .
H13 H 0.1383 0.6407 0.1001 0.028 Uiso 1 1 calc R U
C14 C 0.2373(3) 0.6808(2) 0.1943(2) 0.0170(5) Uani 1 1 d . .
C15 C 0.3674(3) 0.6026(2) 0.1803(2) 0.0166(5) Uani 1 1 d . .
C16 C 0.3998(3) 0.5137(3) 0.1317(2) 0.0215(6) Uani 1 1 d . .
H16 H 0.3401 0.4937 0.0972 0.026 Uiso 1 1 calc R U
C17 C 0.5805(3) 0.5328(2) 0.2145(2) 0.0166(5) Uani 1 1 d . .
C18 C 0.8009(3) 0.4184(3) 0.2399(2) 0.0224(6) Uani 1 1 d . .
H18A H 0.8626 0.4529 0.1661 0.027 Uiso 1 1 calc R U
H18B H 0.7541 0.3364 0.2503 0.027 Uiso 1 1 calc R U
C19 C 0.1782(3) 0.3371(3) 0.4837(3) 0.0305(7) Uani 1 1 d . .
C20 C 0.2710(4) 0.1917(3) 0.1307(3) 0.0334(7) 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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
N5 Cu1 N2 177.71(9) . .
N5 Cu1 N1 99.39(8) . .
N2 Cu1 N1 82.23(9) . .
N5 Cu1 N4 81.17(9) . .
N2 Cu1 N4 99.94(9) . .
N1 Cu1 N4 106.99(9) . .
N5 Cu1 O1 86.13(8) . .
N2 Cu1 O1 91.71(8) . .
N1 Cu1 O1 153.42(9) . .
N4 Cu1 O1 99.54(9) . .
C16 S1 C17 90.32(13) . .
O5 S2 O4 114.64(15) . .
O5 S2 O6 116.10(16) . .
O4 S2 O6 115.10(14) . .
O5 S2 C20 101.98(15) . .
O4 S2 C20 102.70(14) . .
O6 S2 C20 103.54(16) . .
O3 S3 O2 117.18(13) . .
O3 S3 O1 115.48(12) . .
O2 S3 O1 111.86(12) . .
O3 S3 C19 103.97(14) . .
O2 S3 C19 103.72(14) . .
O1 S3 C19 102.26(14) . .
C7 S4 C8 89.97(13) . .
C1 N1 C5 119.0(2) . .
C1 N1 Cu1 127.02(17) . .
C5 N1 Cu1 113.99(17) . .
C8 N2 C6 111.6(2) . .
C8 N2 Cu1 134.65(17) . .
C6 N2 Cu1 113.73(17) . .
C8 N3 C9 125.1(2) . .
C8 N3 H3A 117.4 . .
C9 N3 H3A 117.4 . .
C10 N4 C14 118.7(2) . .
C10 N4 Cu1 128.95(19) . .
C14 N4 Cu1 112.22(18) . .
C17 N5 C15 111.6(2) . .
C17 N5 Cu1 132.11(19) . .
C15 N5 Cu1 114.40(17) . .
C17 N6 C18 120.4(2) . .
C17 N6 H6 119.8 . .
C18 N6 H6 119.8 . .
S3 O1 Cu1 154.01(12) . .
N1 C1 C2 122.4(2) . .
N1 C1 H1 118.8 . .
C2 C1 H1 118.8 . .
C1 C2 C3 118.7(3) . .
C1 C2 H2 120.7 . .
C3 C2 H2 120.7 . .
C4 C3 C2 119.5(3) . .
C4 C3 H3 120.3 . .
C2 C3 H3 120.3 . .
C3 C4 C5 119.2(2) . .
C3 C4 H4 120.4 . .
C5 C4 H4 120.4 . .
N1 C5 C4 121.3(2) . .
N1 C5 C6 114.1(2) . .
C4 C5 C6 124.6(2) . .
C7 C6 N2 115.0(2) . .
C7 C6 C5 129.2(2) . .
N2 C6 C5 115.8(2) . .
C6 C7 S4 110.5(2) . .
C6 C7 H7 124.8 . .
S4 C7 H7 124.8 . .
N2 C8 N3 123.8(2) . .
N2 C8 S4 112.83(19) . .
N3 C8 S4 123.4(2) . .
N3 C9 C18 114.5(2) . 2_666
N3 C9 H9A 108.6 . .
C18 C9 H9A 108.6 2_666 .
N3 C9 H9B 108.6 . .
C18 C9 H9B 108.6 2_666 .
H9A C9 H9B 107.6 . .
N4 C10 C11 122.9(3) . .
N4 C10 H10 118.6 . .
C11 C10 H10 118.6 . .
C10 C11 C12 118.3(3) . .
C10 C11 H11 120.8 . .
C12 C11 H11 120.8 . .
C13 C12 C11 119.7(3) . .
C13 C12 H12 120.2 . .
C11 C12 H12 120.2 . .
C12 C13 C14 118.4(3) . .
C12 C13 H13 120.8 . .
C14 C13 H13 120.8 . .
N4 C14 C13 121.9(3) . .
N4 C14 C15 114.5(2) . .
C13 C14 C15 123.6(2) . .
C16 C15 N5 114.5(2) . .
C16 C15 C14 128.4(3) . .
N5 C15 C14 117.0(2) . .
C15 C16 S1 110.8(2) . .
C15 C16 H16 124.6 . .
S1 C16 H16 124.6 . .
N6 C17 N5 125.6(2) . .
N6 C17 S1 121.62(19) . .
N5 C17 S1 112.8(2) . .
N6 C18 C9 113.2(2) . 2_666
N6 C18 H18A 108.9 . .
C9 C18 H18A 108.9 2_666 .
N6 C18 H18B 108.9 . .
C9 C18 H18B 108.9 2_666 .
H18A C18 H18B 107.8 . .
F1 C19 F3 108.3(3) . .
F1 C19 F2 108.2(3) . .
F3 C19 F2 107.4(2) . .
F1 C19 S3 110.9(2) . .
F3 C19 S3 111.7(2) . .
F2 C19 S3 110.2(2) . .
F4 C20 F6 107.0(3) . .
F4 C20 F5 107.7(3) . .
F6 C20 F5 106.5(3) . .
F4 C20 S2 111.7(2) . .
F6 C20 S2 111.5(2) . .
F5 C20 S2 112.2(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N5 1.948(2) .
Cu1 N2 1.955(2) .
Cu1 N1 2.024(2) .
Cu1 N4 2.126(2) .
Cu1 O1 2.1693(19) .
S1 C16 1.714(3) .
S1 C17 1.739(2) .
S2 O5 1.430(2) .
S2 O4 1.433(2) .
S2 O6 1.438(2) .
S2 C20 1.815(4) .
S3 O3 1.428(2) .
S3 O2 1.437(2) .
S3 O1 1.4579(19) .
S3 C19 1.811(3) .
S4 C7 1.725(3) .
S4 C8 1.740(2) .
F1 C19 1.323(4) .
F2 C19 1.336(4) .
F3 C19 1.325(3) .
F4 C20 1.324(4) .
F5 C20 1.335(4) .
F6 C20 1.329(4) .
N1 C1 1.338(3) .
N1 C5 1.350(3) .
N2 C8 1.328(3) .
N2 C6 1.388(3) .
N3 C8 1.331(3) .
N3 C9 1.465(3) .
N3 H3A 0.8800 .
N4 C10 1.335(4) .
N4 C14 1.348(3) .
N5 C17 1.327(3) .
N5 C15 1.400(3) .
N6 C17 1.324(4) .
N6 C18 1.454(3) .
N6 H6 0.8800 .
C1 C2 1.377(4) .
C1 H1 0.9500 .
C2 C3 1.387(4) .
C2 H2 0.9500 .
C3 C4 1.369(4) .
C3 H3 0.9500 .
C4 C5 1.391(4) .
C4 H4 0.9500 .
C5 C6 1.461(4) .
C6 C7 1.351(3) .
C7 H7 0.9500 .
C9 C18 1.512(4) 2_666
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 C11 1.381(4) .
C10 H10 0.9500 .
C11 C12 1.386(4) .
C11 H11 0.9500 .
C12 C13 1.383(4) .
C12 H12 0.9500 .
C13 C14 1.393(4) .
C13 H13 0.9500 .
C14 C15 1.456(4) .
C15 C16 1.352(3) .
C16 H16 0.9500 .
C18 C9 1.512(4) 2_666
C18 H18A 0.9900 .
C18 H18B 0.9900 .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139188908
