#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:44:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179732 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/28/7002831.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_7002831
loop_
_publ_author_name
'Jin, Jun-Cheng'
'Wang, Yao-Yu'
'Zhang, Wei-Hong'
'Lermontov, Anatoly S.'
'Lermontova, Elmira Kh.'
'Shi, Qi-Zhen'
_publ_section_title
;
 New types of di-, tetra-, hexa- and octanuclear Ag(i) complexes
 containing 1,3-adamantanedicarboxylic acid
;
_journal_issue                   46
_journal_name_full               'Dalton Transactions'
_journal_page_first              10181
_journal_page_last               10191
_journal_paper_doi               10.1039/b909309e
_journal_year                    2009
_chemical_formula_moiety         'C25 H29 Ag N2 O4, C H4 O'
_chemical_formula_sum            'C26 H33 Ag N2 O5'
_chemical_formula_weight         561.41
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 100.159(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4101(10)
_cell_length_b                   9.9258(10)
_cell_length_c                   24.483(3)
_cell_measurement_reflns_used    4468
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.20
_cell_measurement_theta_min      1.69
_cell_volume                     2490.1(5)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        APEX2
_computing_molecular_graphics    APEX2
_computing_publication_material  APEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX SMART II'
_diffrn_measurement_method       ω
_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  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            12516
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         1.69
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_T_max  0.8353
_exptl_absorpt_correction_T_min  0.7730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.820
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.820
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.004
_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+0.6221P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1123
_reflns_number_gt                3698
_reflns_number_total             4468
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b909309e.txt
_cod_data_source_block           081006bjin
_cod_original_cell_volume        2490.2(4)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7002831
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.62163(2) 0.41524(2) 1.008420(9) 0.05126(13) Uani 1 1 d . . .
O3 O 0.5646(2) 0.6545(2) 0.72855(8) 0.0510(5) Uani 1 1 d . . .
O2 O 0.8034(2) 0.4587(2) 0.94793(10) 0.0612(6) Uani 1 1 d . . .
O1 O 0.6597(2) 0.6158(2) 0.95169(10) 0.0592(6) Uani 1 1 d . . .
O4 O 0.7260(2) 0.7324(3) 0.68974(8) 0.0552(6) Uani 1 1 d . . .
H4 H 0.6687 0.7354 0.6621 0.083 Uiso 1 1 calc R . .
C3 C 0.7210(2) 0.6289(3) 0.83343(10) 0.0330(5) Uani 1 1 d . . .
H3A H 0.6322 0.6547 0.8356 0.040 Uiso 1 1 calc R . .
H3B H 0.7214 0.5337 0.8245 0.040 Uiso 1 1 calc R . .
C4 C 0.7687(2) 0.7107(3) 0.78753(10) 0.0345(6) Uani 1 1 d . . .
C2 C 0.8095(2) 0.6540(3) 0.88971(10) 0.0344(6) Uani 1 1 d . . .
C1 C 0.7549(3) 0.5704(3) 0.93355(11) 0.0373(6) Uani 1 1 d . . .
C6 C 0.9093(3) 0.6712(3) 0.78435(12) 0.0406(6) Uani 1 1 d . . .
H6A H 0.9397 0.7232 0.7556 0.049 Uiso 1 1 calc R . .
H6B H 0.9129 0.5765 0.7749 0.049 Uiso 1 1 calc R . .
C7 C 0.7663(3) 0.8620(3) 0.80230(12) 0.0414(6) Uani 1 1 d . . .
H7A H 0.7970 0.9149 0.7738 0.050 Uiso 1 1 calc R . .
H7B H 0.6776 0.8895 0.8038 0.050 Uiso 1 1 calc R . .
C5 C 0.6746(3) 0.6941(3) 0.73312(11) 0.0372(6) Uani 1 1 d . . .
C12 C 0.9494(3) 0.6145(3) 0.88561(12) 0.0411(6) Uani 1 1 d . . .
H12A H 0.9527 0.5195 0.8768 0.049 Uiso 1 1 calc R . .
H12B H 1.0059 0.6297 0.9210 0.049 Uiso 1 1 calc R . .
C10 C 0.8529(3) 0.8876(3) 0.85803(13) 0.0460(7) Uani 1 1 d . . .
H10 H 0.8504 0.9837 0.8671 0.055 Uiso 1 1 calc R . .
C11 C 0.8045(3) 0.8055(3) 0.90305(11) 0.0426(6) Uani 1 1 d . . .
H11A H 0.7156 0.8313 0.9051 0.051 Uiso 1 1 calc R . .
H11B H 0.8587 0.8237 0.9387 0.051 Uiso 1 1 calc R . .
C8 C 0.9975(3) 0.6979(3) 0.84057(13) 0.0448(7) Uani 1 1 d . . .
H8 H 1.0873 0.6719 0.8385 0.054 Uiso 1 1 calc R . .
C9 C 0.9934(3) 0.8472(3) 0.85470(14) 0.0525(8) Uani 1 1 d . . .
H9A H 1.0246 0.9001 0.8264 0.063 Uiso 1 1 calc R . .
H9B H 1.0497 0.8646 0.8900 0.063 Uiso 1 1 calc R . .
N1 N 0.6729(2) 0.5060(2) 1.09190(9) 0.0412(5) Uani 1 1 d . . .
C13 C 0.7745(3) 0.5872(3) 1.10606(14) 0.0458(7) Uani 1 1 d . . .
H13 H 0.8246 0.6080 1.0793 0.055 Uiso 1 1 calc R . .
C15 C 0.7382(3) 0.6135(3) 1.19853(12) 0.0409(6) Uani 1 1 d . . .
C14 C 0.8097(3) 0.6420(3) 1.15768(12) 0.0453(7) Uani 1 1 d . . .
H14 H 0.8820 0.6985 1.1653 0.054 Uiso 1 1 calc R . .
C18 C 0.7780(3) 0.6631(3) 1.25709(12) 0.0476(7) Uani 1 1 d . . .
H18A H 0.7037 0.7047 1.2693 0.057 Uiso 1 1 calc R . .
H18B H 0.8456 0.7308 1.2583 0.057 Uiso 1 1 calc R . .
C17 C 0.6022(3) 0.4798(3) 1.13107(13) 0.0498(7) Uani 1 1 d . . .
H17 H 0.5297 0.4241 1.1221 0.060 Uiso 1 1 calc R . .
C16 C 0.6304(3) 0.5304(3) 1.18366(12) 0.0501(7) Uani 1 1 d . . .
H16 H 0.5777 0.5093 1.2094 0.060 Uiso 1 1 calc R . .
N2 N 0.5359(2) 0.2401(2) 0.95938(10) 0.0464(6) Uani 1 1 d . . .
C26 C 0.4349(3) 0.0232(3) 0.89198(12) 0.0431(6) Uani 1 1 d . . .
C25 C 0.3830(3) 0.0619(3) 0.93770(13) 0.0495(7) Uani 1 1 d . . .
H25 H 0.3123 0.0152 0.9469 0.059 Uiso 1 1 calc R . .
C27 C 0.5382(4) 0.0983(3) 0.88092(16) 0.0589(9) Uani 1 1 d . . .
H27 H 0.5760 0.0778 0.8502 0.071 Uiso 1 1 calc R . .
C24 C 0.4352(3) 0.1687(3) 0.96973(13) 0.0522(8) Uani 1 1 d . . .
H24 H 0.3980 0.1923 1.0003 0.063 Uiso 1 1 calc R . .
C28 C 0.5858(3) 0.2034(4) 0.91494(14) 0.0595(9) Uani 1 1 d . . .
H28 H 0.6565 0.2517 0.9066 0.071 Uiso 1 1 calc R . .
C30 C 0.8807(3) 0.5925(3) 1.35534(13) 0.0485(7) Uani 1 1 d . . .
H30A H 0.9488 0.6591 1.3550 0.058 Uiso 1 1 calc R . .
H30B H 0.8109 0.6348 1.3706 0.058 Uiso 1 1 calc R . .
C29 C 0.8286(3) 0.5478(3) 1.29612(13) 0.0508(7) Uani 1 1 d . . .
H29A H 0.7584 0.4838 1.2966 0.061 Uiso 1 1 calc R . .
H29B H 0.8977 0.5017 1.2817 0.061 Uiso 1 1 calc R . .
O5 O 0.9245(2) 0.2652(2) 0.90691(9) 0.0579(6) Uani 1 1 d . . .
H5 H 0.8897 0.3302 0.9189 0.087 Uiso 1 1 calc R . .
C31 C 0.9778(6) 0.1832(5) 0.95020(19) 0.1007(17) Uani 1 1 d . . .
H31A H 1.0347 0.2352 0.9774 0.151 Uiso 1 1 calc R . .
H31B H 1.0267 0.1125 0.9367 0.151 Uiso 1 1 calc R . .
H31C H 0.9093 0.1447 0.9668 0.151 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
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'
Ag Ag -0.8971 1.1015 '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'
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
_geom_angle_publ_flag
N2 Ag1 N1 146.22(9) . . ?
N2 Ag1 O1 114.41(9) . . ?
N1 Ag1 O1 98.82(9) . . ?
N2 Ag1 Ag1 96.66(7) . 3_667 ?
N1 Ag1 Ag1 87.65(6) . 3_667 ?
O1 Ag1 Ag1 71.95(5) . 3_667 ?
C1 O1 Ag1 97.15(18) . . ?
C5 O4 H4 109.5 . . ?
C2 C3 C4 110.5(2) . . ?
C2 C3 H3A 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
C5 C4 C6 113.7(2) . . ?
C5 C4 C3 110.1(2) . . ?
C6 C4 C3 109.7(2) . . ?
C5 C4 C7 106.1(2) . . ?
C6 C4 C7 108.4(2) . . ?
C3 C4 C7 108.7(2) . . ?
C12 C2 C3 109.1(2) . . ?
C12 C2 C11 109.4(2) . . ?
C3 C2 C11 108.1(2) . . ?
C12 C2 C1 112.3(2) . . ?
C3 C2 C1 107.5(2) . . ?
C11 C2 C1 110.3(2) . . ?
O1 C1 O2 122.2(3) . . ?
O1 C1 C2 118.0(2) . . ?
O2 C1 C2 119.7(2) . . ?
C4 C6 C8 109.6(2) . . ?
C4 C6 H6A 109.7 . . ?
C8 C6 H6A 109.7 . . ?
C4 C6 H6B 109.7 . . ?
C8 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
C10 C7 C4 110.0(2) . . ?
C10 C7 H7A 109.7 . . ?
C4 C7 H7A 109.7 . . ?
C10 C7 H7B 109.7 . . ?
C4 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
O3 C5 O4 122.2(3) . . ?
O3 C5 C4 125.2(2) . . ?
O4 C5 C4 112.6(2) . . ?
C2 C12 C8 110.2(2) . . ?
C2 C12 H12A 109.6 . . ?
C8 C12 H12A 109.6 . . ?
C2 C12 H12B 109.6 . . ?
C8 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
C7 C10 C11 109.9(2) . . ?
C7 C10 C9 109.2(3) . . ?
C11 C10 C9 109.8(3) . . ?
C7 C10 H10 109.3 . . ?
C11 C10 H10 109.3 . . ?
C9 C10 H10 109.3 . . ?
C10 C11 C2 109.9(2) . . ?
C10 C11 H11A 109.7 . . ?
C2 C11 H11A 109.7 . . ?
C10 C11 H11B 109.7 . . ?
C2 C11 H11B 109.7 . . ?
H11A C11 H11B 108.2 . . ?
C9 C8 C12 109.6(3) . . ?
C9 C8 C6 109.6(2) . . ?
C12 C8 C6 109.4(2) . . ?
C9 C8 H8 109.4 . . ?
C12 C8 H8 109.4 . . ?
C6 C8 H8 109.4 . . ?
C8 C9 C10 109.4(2) . . ?
C8 C9 H9A 109.8 . . ?
C10 C9 H9A 109.8 . . ?
C8 C9 H9B 109.8 . . ?
C10 C9 H9B 109.8 . . ?
H9A C9 H9B 108.2 . . ?
C13 N1 C17 116.5(3) . . ?
C13 N1 Ag1 122.7(2) . . ?
C17 N1 Ag1 120.8(2) . . ?
N1 C13 C14 123.7(3) . . ?
N1 C13 H13 118.1 . . ?
C14 C13 H13 118.1 . . ?
C14 C15 C16 116.5(3) . . ?
C14 C15 C18 122.1(3) . . ?
C16 C15 C18 121.2(3) . . ?
C13 C14 C15 119.9(3) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C15 C18 C29 111.1(2) . . ?
C15 C18 H18A 109.4 . . ?
C29 C18 H18A 109.4 . . ?
C15 C18 H18B 109.4 . . ?
C29 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
N1 C17 C16 123.5(3) . . ?
N1 C17 H17 118.2 . . ?
C16 C17 H17 118.2 . . ?
C17 C16 C15 119.7(3) . . ?
C17 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C24 N2 C28 116.4(3) . . ?
C24 N2 Ag1 125.0(2) . . ?
C28 N2 Ag1 118.6(2) . . ?
C27 C26 C25 116.2(3) . . ?
C27 C26 C30 121.4(3) . 4_565 ?
C25 C26 C30 122.5(3) . 4_565 ?
C24 C25 C26 120.4(3) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C28 C27 C26 120.3(3) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
N2 C24 C25 123.4(3) . . ?
N2 C24 H24 118.3 . . ?
C25 C24 H24 118.3 . . ?
N2 C28 C27 123.4(3) . . ?
N2 C28 H28 118.3 . . ?
C27 C28 H28 118.3 . . ?
C26 C30 C29 112.3(2) 4_666 . ?
C26 C30 H30A 109.2 4_666 . ?
C29 C30 H30A 109.2 . . ?
C26 C30 H30B 109.2 4_666 . ?
C29 C30 H30B 109.2 . . ?
H30A C30 H30B 107.9 . . ?
C30 C29 C18 113.9(3) . . ?
C30 C29 H29A 108.8 . . ?
C18 C29 H29A 108.8 . . ?
C30 C29 H29B 108.8 . . ?
C18 C29 H29B 108.8 . . ?
H29A C29 H29B 107.7 . . ?
C31 O5 H5 109.5 . . ?
O5 C31 H31A 109.5 . . ?
O5 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
O5 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 N2 2.210(2) . ?
Ag1 N1 2.211(2) . ?
Ag1 O1 2.499(2) . ?
Ag1 Ag1 3.0076(5) 3_667 ?
O3 C5 1.198(3) . ?
O2 C1 1.243(4) . ?
O1 C1 1.240(4) . ?
O4 C5 1.326(3) . ?
O4 H4 0.8200 . ?
C3 C2 1.537(4) . ?
C3 C4 1.537(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.517(4) . ?
C4 C6 1.531(4) . ?
C4 C7 1.546(4) . ?
C2 C12 1.528(4) . ?
C2 C11 1.541(4) . ?
C2 C1 1.543(4) . ?
C6 C8 1.537(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C10 1.518(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C12 C8 1.531(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C10 C11 1.527(4) . ?
C10 C9 1.532(5) . ?
C10 H10 0.9800 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C8 C9 1.524(5) . ?
C8 H8 0.9800 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
N1 C13 1.327(4) . ?
N1 C17 1.334(4) . ?
C13 C14 1.365(4) . ?
C13 H13 0.9300 . ?
C15 C14 1.377(4) . ?
C15 C16 1.388(4) . ?
C15 C18 1.503(4) . ?
C14 H14 0.9300 . ?
C18 C29 1.524(4) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C17 C16 1.365(4) . ?
C17 H17 0.9300 . ?
C16 H16 0.9300 . ?
N2 C24 1.326(4) . ?
N2 C28 1.336(4) . ?
C26 C27 1.374(5) . ?
C26 C25 1.380(4) . ?
C26 C30 1.504(4) 4_565 ?
C25 C24 1.373(5) . ?
C25 H25 0.9300 . ?
C27 C28 1.372(5) . ?
C27 H27 0.9300 . ?
C24 H24 0.9300 . ?
C28 H28 0.9300 . ?
C30 C26 1.504(4) 4_666 ?
C30 C29 1.522(4) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
O5 C31 1.373(5) . ?
O5 H5 0.8200 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
