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#$Date: 2019-11-17 08:33:25 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228879 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/08/7230878.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_7230878
loop_
_publ_author_name
'Xu, Lin-Yan'
'Yang, Wei'
'Liu, Chao-Fan'
'Ren, Zhi-Gang'
'Lang, Jian-Ping'
_publ_section_title
;
 Assembly of silver-oxo complexes based on
 N-diphenylphosphanylmethyl-3-aminopyridine and their structures,
 photocatalysis and photocurrent responses
;
_journal_issue                   28
_journal_name_full               CrystEngComm
_journal_page_first              4049
_journal_paper_doi               10.1039/C8CE00715B
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C38 H34 Ag2 F6 N4 O6 P2 S2'
_chemical_formula_sum            'C38 H34 Ag2 F6 N4 O6 P2 S2'
_chemical_formula_weight         1098.49
_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-2016/6
_audit_update_record
;
2018-05-31 deposited with the CCDC.
2018-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                104.48(3)
_cell_angle_beta                 106.68(3)
_cell_angle_gamma                105.64(3)
_cell_formula_units_Z            1
_cell_length_a                   9.3658(19)
_cell_length_b                   10.897(2)
_cell_length_c                   12.166(2)
_cell_measurement_reflns_used    229
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      34.9725
_cell_measurement_theta_min      2.4422
_cell_volume                     1070.8(5)
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction        'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       /w
_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  0.0259
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8499
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.442
_exptl_absorpt_coefficient_mu    1.162
_exptl_absorpt_correction_T_max  0.793
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.157
_refine_diff_density_min         -3.852
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3738
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1168
_refine_ls_R_factor_gt           0.1132
_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)+(0.2530P)²+5.2000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3334
_refine_ls_wR_factor_ref         0.3401
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3478
_reflns_number_total             3773
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce00715b2.cif
_cod_data_source_block           a_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7230876--7230881.cif.'
_cod_database_code               7230878
_shelx_shelxl_version_number     2016/6
_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.
;
_shelx_estimated_absorpt_t_min   0.801
_shelx_estimated_absorpt_t_max   0.801
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
Ag1 Ag 0.46997(10) 0.27972(8) 0.47890(9) 0.0673(5) Uani 1 1 d . .
P1 P 0.6605(3) 0.2054(2) 0.4202(2) 0.0449(6) Uani 1 1 d . .
N1 N 0.8061(11) 0.3857(8) 0.3216(8) 0.058(2) Uani 1 1 d . .
H1 H 0.829666 0.348770 0.261391 0.069 Uiso 1 1 calc R U
N2 N 0.6271(10) 0.6390(8) 0.3876(7) 0.0504(17) Uani 1 1 d . .
C1 C 0.8375(11) 0.3400(9) 0.4238(10) 0.051(2) Uani 1 1 d . .
H1A H 0.876209 0.417818 0.498761 0.061 Uiso 1 1 calc R U
H1B H 0.922559 0.304563 0.426535 0.061 Uiso 1 1 calc R U
C2 C 0.7417(10) 0.4835(9) 0.3119(8) 0.0464(19) Uani 1 1 d . .
C3 C 0.7227(15) 0.5232(11) 0.2086(10) 0.064(3) Uani 1 1 d . .
H3 H 0.754465 0.483905 0.147260 0.076 Uiso 1 1 calc R U
C4 C 0.6587(16) 0.6178(12) 0.1992(10) 0.066(3) Uani 1 1 d . .
H4 H 0.650127 0.646048 0.132343 0.079 Uiso 1 1 calc R U
C5 C 0.6054(15) 0.6741(12) 0.2858(11) 0.067(3) Uani 1 1 d . .
H5 H 0.554981 0.735487 0.275180 0.080 Uiso 1 1 calc R U
C6 C 0.6924(10) 0.5472(9) 0.3990(8) 0.0465(19) Uani 1 1 d . .
H6 H 0.705661 0.524321 0.469017 0.056 Uiso 1 1 calc R U
C7 C 0.7652(11) 0.1484(9) 0.5372(8) 0.0477(19) Uani 1 1 d . .
C8 C 0.8261(16) 0.2324(12) 0.6612(12) 0.074(3) Uani 1 1 d . .
H8 H 0.806375 0.312723 0.680554 0.089 Uiso 1 1 calc R U
C9 C 0.9094(15) 0.2034(14) 0.7513(10) 0.069(3) Uani 1 1 d . .
H9 H 0.948069 0.261387 0.832473 0.083 Uiso 1 1 calc R U
C10 C 0.9383(16) 0.0796(15) 0.7201(13) 0.078(3) Uani 1 1 d . .
H10 H 0.997917 0.056495 0.781635 0.093 Uiso 1 1 calc R U
C11 C 0.8787(15) -0.0057(13) 0.5997(12) 0.069(3) Uani 1 1 d . .
H11 H 0.898883 -0.085774 0.580269 0.082 Uiso 1 1 calc R U
C12 C 0.7904(13) 0.0262(10) 0.5090(10) 0.058(2) Uani 1 1 d . .
H12 H 0.746971 -0.033624 0.428077 0.069 Uiso 1 1 calc R U
C13 C 0.5943(12) 0.0692(9) 0.2731(8) 0.049(2) Uani 1 1 d . .
C14 C 0.4342(14) -0.0082(12) 0.2172(12) 0.072(3) Uani 1 1 d . .
H14 H 0.362649 0.009236 0.252646 0.086 Uiso 1 1 calc R U
C15 C 0.380(2) -0.1166(15) 0.1028(14) 0.095(5) Uani 1 1 d . .
H15 H 0.271134 -0.169296 0.062189 0.114 Uiso 1 1 calc R U
C16 C 0.4832(19) -0.1434(13) 0.0532(11) 0.080(4) Uani 1 1 d . .
H16 H 0.446984 -0.216228 -0.019867 0.096 Uiso 1 1 calc R U
C17 C 0.6400(18) -0.0645(13) 0.1095(11) 0.074(3) Uani 1 1 d . .
H17 H 0.710506 -0.082200 0.072929 0.089 Uiso 1 1 calc R U
C18 C 0.6993(14) 0.0422(11) 0.2204(9) 0.058(2) Uani 1 1 d . .
H18 H 0.808272 0.094673 0.258511 0.069 Uiso 1 1 calc R U
S1 S 0.1549(4) 0.3352(3) 0.2445(3) 0.0725(8) Uani 1 1 d . U
O1 O 0.1796(12) 0.2443(9) 0.3026(8) 0.0777(10) Uani 1 1 d . U
O2 O -0.0197(12) 0.3070(9) 0.1732(8) 0.0771(10) Uani 1 1 d . U
O3 O 0.2367(12) 0.4735(9) 0.3151(8) 0.0762(10) Uani 1 1 d . U
C19 C 0.203(2) 0.290(3) 0.1148(16) 0.128(5) Uani 1 1 d . U
F1 F 0.233(3) 0.374(3) 0.0654(17) 0.244(7) Uani 1 1 d . U
F2 F 0.1138(19) 0.180(2) 0.0336(13) 0.213(7) Uani 1 1 d . U
F3 F 0.359(2) 0.289(3) 0.1587(18) 0.278(11) Uani 1 1 d . U
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'
Ag Ag -0.8971 1.1015 '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'
P P 0.1023 0.0942 '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'
F F 0.0171 0.0103 '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
N2 Ag1 P1 154.0(2) 2_666 .
C13 P1 C7 106.3(4) . .
C13 P1 C1 104.3(5) . .
C7 P1 C1 99.0(4) . .
C13 P1 Ag1 119.4(3) . .
C7 P1 Ag1 108.9(3) . .
C1 P1 Ag1 116.6(3) . .
C2 N1 C1 125.4(8) . .
C2 N1 H1 117.3 . .
C1 N1 H1 117.3 . .
C6 N2 C5 119.9(9) . .
C6 N2 Ag1 120.7(6) . 2_666
C5 N2 Ag1 119.1(7) . 2_666
N1 C1 P1 114.8(7) . .
N1 C1 H1A 108.6 . .
P1 C1 H1A 108.6 . .
N1 C1 H1B 108.6 . .
P1 C1 H1B 108.6 . .
H1A C1 H1B 107.5 . .
N1 C2 C6 123.5(9) . .
N1 C2 C3 119.9(9) . .
C6 C2 C3 116.6(9) . .
C4 C3 C2 119.6(10) . .
C4 C3 H3 120.2 . .
C2 C3 H3 120.2 . .
C3 C4 C5 121.6(10) . .
C3 C4 H4 119.2 . .
C5 C4 H4 119.2 . .
N2 C5 C4 119.1(10) . .
N2 C5 H5 120.4 . .
C4 C5 H5 120.4 . .
N2 C6 C2 123.1(9) . .
N2 C6 H6 118.5 . .
C2 C6 H6 118.5 . .
C12 C7 C8 118.1(10) . .
C12 C7 P1 122.9(7) . .
C8 C7 P1 119.0(8) . .
C9 C8 C7 123.5(12) . .
C9 C8 H8 118.3 . .
C7 C8 H8 118.3 . .
C8 C9 C10 117.6(11) . .
C8 C9 H9 121.2 . .
C10 C9 H9 121.2 . .
C11 C10 C9 120.4(11) . .
C11 C10 H10 119.8 . .
C9 C10 H10 119.8 . .
C12 C11 C10 120.5(11) . .
C12 C11 H11 119.8 . .
C10 C11 H11 119.8 . .
C11 C12 C7 119.9(10) . .
C11 C12 H12 120.1 . .
C7 C12 H12 120.1 . .
C14 C13 C18 120.5(10) . .
C14 C13 P1 117.1(9) . .
C18 C13 P1 122.3(8) . .
C13 C14 C15 118.1(13) . .
C13 C14 H14 120.9 . .
C15 C14 H14 120.9 . .
C16 C15 C14 120.9(13) . .
C16 C15 H15 119.6 . .
C14 C15 H15 119.6 . .
C15 C16 C17 119.8(12) . .
C15 C16 H16 120.1 . .
C17 C16 H16 120.1 . .
C16 C17 C18 121.8(13) . .
C16 C17 H17 119.1 . .
C18 C17 H17 119.1 . .
C13 C18 C17 118.9(11) . .
C13 C18 H18 120.6 . .
C17 C18 H18 120.6 . .
O1 S1 O3 116.6(6) . .
O1 S1 O2 114.7(6) . .
O3 S1 O2 110.6(6) . .
O1 S1 C19 106.0(10) . .
O3 S1 C19 111.4(9) . .
O2 S1 C19 95.4(7) . .
F1 C19 F2 108(2) . .
F1 C19 F3 97(2) . .
F2 C19 F3 109(2) . .
F1 C19 S1 119(2) . .
F2 C19 S1 116.5(17) . .
F3 C19 S1 105.6(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 N2 2.194(8) 2_666
Ag1 P1 2.360(2) .
P1 C13 1.824(9) .
P1 C7 1.828(9) .
P1 C1 1.876(9) .
N1 C2 1.371(13) .
N1 C1 1.435(13) .
N1 H1 0.8600 .
N2 C6 1.321(12) .
N2 C5 1.362(14) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 C6 1.380(13) .
C2 C3 1.408(14) .
C3 C4 1.337(18) .
C3 H3 0.9300 .
C4 C5 1.371(18) .
C4 H4 0.9300 .
C5 H5 0.9300 .
C6 H6 0.9300 .
C7 C12 1.392(14) .
C7 C8 1.405(15) .
C8 C9 1.313(19) .
C8 H8 0.9300 .
C9 C10 1.43(2) .
C9 H9 0.9300 .
C10 C11 1.375(19) .
C10 H10 0.9300 .
C11 C12 1.358(16) .
C11 H11 0.9300 .
C12 H12 0.9300 .
C13 C14 1.367(15) .
C13 C18 1.375(15) .
C14 C15 1.428(19) .
C14 H14 0.9300 .
C15 C16 1.34(2) .
C15 H15 0.9300 .
C16 C17 1.35(2) .
C16 H16 0.9300 .
C17 C18 1.385(15) .
C17 H17 0.9300 .
C18 H18 0.9300 .
S1 O1 1.385(10) .
S1 O3 1.395(9) .
S1 O2 1.517(11) .
S1 C19 1.752(18) .
C19 F1 1.23(3) .
C19 F2 1.23(2) .
C19 F3 1.41(3) .
