#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:32:06 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179900 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/96/7019631.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_7019631
loop_
_publ_author_name
'Sun, Sha'
'Ren, Zhi-Gang'
'Yang, Ju-Hua'
'He, Run-Tian'
'Wang, Fan'
'Wu, Xin-Yi'
'Gong, Wei-Jie'
'Li, Hong-Xi'
'Lang, Jian-Ping'
_publ_section_title
;
 Formation of N-heterocyclic diphosphine ligands from Ag(i)-assisted
 condensation reactions between bdppeda and formaldehyde and their
 binuclear silver(i) complexes.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8447
_journal_page_last               8454
_journal_paper_doi               10.1039/c2dt30860f
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C58 H60 Ag2 Cl2 N4 P4, 2(C H4 O)'
_chemical_formula_sum            'C60 H68 Ag2 Cl2 N4 O2 P4'
_chemical_formula_weight         1287.70
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_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
_cell_angle_alpha                109.74(3)
_cell_angle_beta                 98.42(3)
_cell_angle_gamma                91.44(3)
_cell_formula_units_Z            1
_cell_length_a                   9.814(2)
_cell_length_b                   11.780(2)
_cell_length_c                   13.337(3)
_cell_measurement_reflns_used    6668
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.4971
_cell_measurement_theta_min      3.1682
_cell_volume                     1431.0(6)
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction
'CrystalStructure, Ver. 3.60 (Rigaku/MSC,2004)'
_computing_molecular_graphics    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13124
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.29
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.936
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7447
_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    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         6420
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0346
_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)+(0.0398P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0796
_reflns_number_gt                5471
_reflns_number_total             6420
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30860f.txt
_cod_data_source_block           3^.^2CH^3^OH
_cod_original_cell_volume        1431.0(5)
_cod_database_code               7019631
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
Ag1 Ag 0.536443(18) 0.633722(17) 0.624361(14) 0.03023(7) Uani 1 1 d .
P1 P 0.76537(6) 0.67467(6) 0.73935(5) 0.02553(14) Uani 1 1 d .
P2 P 0.65153(6) 0.23178(6) 0.33481(5) 0.02676(14) Uani 1 1 d .
Cl1 Cl 0.38466(6) 0.42452(5) 0.56974(4) 0.03262(14) Uani 1 1 d .
N1 N 0.8607(2) 0.44926(19) 0.69100(15) 0.0299(5) Uani 1 1 d .
N2 N 0.8506(2) 0.2955(2) 0.51843(15) 0.0329(5) Uani 1 1 d .
C1 C 0.8974(2) 0.5708(2) 0.69039(19) 0.0295(5) Uani 1 1 d .
H1A H 0.9060 0.5659 0.6168 0.035 Uiso 1 1 calc R
H1B H 0.9870 0.6023 0.7366 0.035 Uiso 1 1 calc R
C2 C 0.9824(3) 0.3777(3) 0.6884(2) 0.0410(7) Uani 1 1 d .
H2A H 0.9675 0.3120 0.7161 0.049 Uiso 1 1 calc R
H2B H 1.0652 0.4289 0.7316 0.049 Uiso 1 1 calc R
C3 C 0.9969(3) 0.3279(3) 0.5706(2) 0.0429(7) Uani 1 1 d .
H3A H 1.0401 0.3890 0.5479 0.052 Uiso 1 1 calc R
H3B H 1.0506 0.2567 0.5551 0.052 Uiso 1 1 calc R
C4 C 0.7665(3) 0.3750(2) 0.59125(19) 0.0335(6) Uani 1 1 d .
H4A H 0.6972 0.3265 0.6088 0.040 Uiso 1 1 calc R
H4B H 0.7185 0.4274 0.5566 0.040 Uiso 1 1 calc R
C5 C 0.8278(3) 0.2922(3) 0.40795(19) 0.0344(6) Uani 1 1 d .
H5A H 0.8949 0.2420 0.3694 0.041 Uiso 1 1 calc R
H5B H 0.8447 0.3743 0.4075 0.041 Uiso 1 1 calc R
C6 C 0.8464(2) 0.8182(2) 0.74357(19) 0.0293(5) Uani 1 1 d .
C7 C 0.9390(3) 0.8919(3) 0.8321(2) 0.0403(6) Uani 1 1 d .
H7 H 0.9664 0.8661 0.8909 0.048 Uiso 1 1 calc R
C8 C 0.9911(3) 1.0027(3) 0.8345(2) 0.0503(8) Uani 1 1 d .
H8 H 1.0534 1.0520 0.8950 0.060 Uiso 1 1 calc R
C9 C 0.9526(3) 1.0416(3) 0.7489(2) 0.0508(8) Uani 1 1 d .
H9 H 0.9867 1.1180 0.7515 0.061 Uiso 1 1 calc R
C10 C 0.8637(3) 0.9677(3) 0.6591(2) 0.0503(8) Uani 1 1 d .
H10 H 0.8391 0.9929 0.5996 0.060 Uiso 1 1 calc R
C11 C 0.8108(3) 0.8569(3) 0.6567(2) 0.0387(6) Uani 1 1 d .
H11 H 0.7501 0.8072 0.5954 0.046 Uiso 1 1 calc R
C12 C 0.7788(2) 0.6900(2) 0.88124(18) 0.0284(5) Uani 1 1 d .
C13 C 0.6747(3) 0.7440(2) 0.9361(2) 0.0348(6) Uani 1 1 d .
H13 H 0.6012 0.7722 0.8997 0.042 Uiso 1 1 calc R
C14 C 0.6769(3) 0.7572(3) 1.0438(2) 0.0424(7) Uani 1 1 d .
H14 H 0.6068 0.7957 1.0805 0.051 Uiso 1 1 calc R
C15 C 0.7839(3) 0.7130(3) 1.0967(2) 0.0426(7) Uani 1 1 d .
H15 H 0.7847 0.7191 1.1689 0.051 Uiso 1 1 calc R
C16 C 0.8878(3) 0.6607(3) 1.0440(2) 0.0438(7) Uani 1 1 d .
H16 H 0.9606 0.6321 1.0807 0.053 Uiso 1 1 calc R
C17 C 0.8872(3) 0.6492(3) 0.9367(2) 0.0360(6) Uani 1 1 d .
H17 H 0.9599 0.6139 0.9015 0.043 Uiso 1 1 calc R
C18 C 0.6339(3) 0.0792(2) 0.33739(19) 0.0344(6) Uani 1 1 d .
C19 C 0.5023(4) 0.0193(3) 0.3051(3) 0.0648(10) Uani 1 1 d .
H19 H 0.4280 0.0574 0.2808 0.078 Uiso 1 1 calc R
C20 C 0.4793(5) -0.0961(4) 0.3085(4) 0.0846(13) Uani 1 1 d .
H20 H 0.3906 -0.1367 0.2847 0.102 Uiso 1 1 calc R
C21 C 0.5864(6) -0.1505(3) 0.3467(3) 0.0790(13) Uani 1 1 d .
H21 H 0.5700 -0.2260 0.3540 0.095 Uiso 1 1 calc R
C22 C 0.7153(5) -0.0957(3) 0.3739(3) 0.0739(12) Uani 1 1 d .
H22 H 0.7892 -0.1353 0.3967 0.089 Uiso 1 1 calc R
C23 C 0.7405(4) 0.0193(3) 0.3686(3) 0.0573(9) Uani 1 1 d .
H23 H 0.8312 0.0557 0.3865 0.069 Uiso 1 1 calc R
C24 C 0.6809(2) 0.2162(2) 0.19884(19) 0.0309(5) Uani 1 1 d .
C25 C 0.6805(3) 0.1055(3) 0.1171(2) 0.0443(7) Uani 1 1 d .
H25 H 0.6655 0.0332 0.1305 0.053 Uiso 1 1 calc R
C26 C 0.7021(4) 0.1016(3) 0.0152(2) 0.0579(9) Uani 1 1 d .
H26 H 0.6997 0.0266 -0.0404 0.069 Uiso 1 1 calc R
C27 C 0.7270(3) 0.2065(3) -0.0045(2) 0.0551(9) Uani 1 1 d .
H27 H 0.7446 0.2028 -0.0729 0.066 Uiso 1 1 calc R
C28 C 0.7264(3) 0.3173(3) 0.0752(2) 0.0476(7) Uani 1 1 d .
H28 H 0.7426 0.3890 0.0611 0.057 Uiso 1 1 calc R
C29 C 0.7017(3) 0.3227(3) 0.1768(2) 0.0378(6) Uani 1 1 d .
H29 H 0.6990 0.3982 0.2308 0.045 Uiso 1 1 calc R
C30 C 0.5970(4) 0.4183(4) 0.8552(3) 0.0675(10) Uani 1 1 d .
H30A H 0.6140 0.4964 0.9128 0.101 Uiso 1 1 calc R
H30B H 0.5401 0.3644 0.8762 0.101 Uiso 1 1 calc R
H30C H 0.5496 0.4283 0.7900 0.101 Uiso 1 1 calc R
O1 O 0.7242(3) 0.3686(2) 0.83597(18) 0.0672(7) Uani 1 1 d .
H1O1 H 0.7569 0.4058 0.7991 0.101 Uiso 1 1 d 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'
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'
Cl Cl 0.1484 0.1585 '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'
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
P1 Ag1 P2 122.79(3) . 2_666
P1 Ag1 Cl1 122.47(3) . .
P2 Ag1 Cl1 97.38(3) 2_666 .
P1 Ag1 Cl1 99.39(3) . 2_666
P2 Ag1 Cl1 119.36(3) 2_666 2_666
Cl1 Ag1 Cl1 92.89(4) . 2_666
C12 P1 C6 103.82(11) . .
C12 P1 C1 104.00(12) . .
C6 P1 C1 101.04(11) . .
C12 P1 Ag1 119.61(8) . .
C6 P1 Ag1 109.45(8) . .
C1 P1 Ag1 116.68(8) . .
C18 P2 C24 106.04(12) . .
C18 P2 C5 104.88(13) . .
C24 P2 C5 98.22(11) . .
C18 P2 Ag1 120.27(9) . 2_666
C24 P2 Ag1 107.33(9) . 2_666
C5 P2 Ag1 117.37(10) . 2_666
Ag1 Cl1 Ag1 87.11(4) . 2_666
C1 N1 C2 111.5(2) . .
C1 N1 C4 112.17(18) . .
C2 N1 C4 102.5(2) . .
C5 N2 C4 116.5(2) . .
C5 N2 C3 112.7(2) . .
C4 N2 C3 107.21(19) . .
N1 C1 P1 110.94(16) . .
N1 C1 H1A 109.5 . .
P1 C1 H1A 109.5 . .
N1 C1 H1B 109.5 . .
P1 C1 H1B 109.5 . .
H1A C1 H1B 108.0 . .
N1 C2 C3 104.59(19) . .
N1 C2 H2A 110.8 . .
C3 C2 H2A 110.8 . .
N1 C2 H2B 110.8 . .
C3 C2 H2B 110.8 . .
H2A C2 H2B 108.9 . .
N2 C3 C2 101.3(2) . .
N2 C3 H3A 111.5 . .
C2 C3 H3A 111.5 . .
N2 C3 H3B 111.5 . .
C2 C3 H3B 111.5 . .
H3A C3 H3B 109.3 . .
N2 C4 N1 107.79(19) . .
N2 C4 H4A 110.1 . .
N1 C4 H4A 110.1 . .
N2 C4 H4B 110.1 . .
N1 C4 H4B 110.1 . .
H4A C4 H4B 108.5 . .
N2 C5 P2 113.70(18) . .
N2 C5 H5A 108.8 . .
P2 C5 H5A 108.8 . .
N2 C5 H5B 108.8 . .
P2 C5 H5B 108.8 . .
H5A C5 H5B 107.7 . .
C11 C6 C7 118.6(2) . .
C11 C6 P1 118.90(18) . .
C7 C6 P1 122.51(19) . .
C8 C7 C6 120.5(2) . .
C8 C7 H7 119.7 . .
C6 C7 H7 119.7 . .
C9 C8 C7 120.5(3) . .
C9 C8 H8 119.8 . .
C7 C8 H8 119.8 . .
C8 C9 C10 119.6(3) . .
C8 C9 H9 120.2 . .
C10 C9 H9 120.2 . .
C9 C10 C11 120.1(3) . .
C9 C10 H10 120.0 . .
C11 C10 H10 120.0 . .
C10 C11 C6 120.7(2) . .
C10 C11 H11 119.6 . .
C6 C11 H11 119.6 . .
C13 C12 C17 118.6(2) . .
C13 C12 P1 117.95(18) . .
C17 C12 P1 123.5(2) . .
C12 C13 C14 121.2(2) . .
C12 C13 H13 119.4 . .
C14 C13 H13 119.4 . .
C13 C14 C15 119.3(3) . .
C13 C14 H14 120.3 . .
C15 C14 H14 120.3 . .
C16 C15 C14 120.1(2) . .
C16 C15 H15 119.9 . .
C14 C15 H15 119.9 . .
C15 C16 C17 120.7(3) . .
C15 C16 H16 119.6 . .
C17 C16 H16 119.6 . .
C16 C17 C12 120.1(3) . .
C16 C17 H17 120.0 . .
C12 C17 H17 120.0 . .
C23 C18 C19 118.0(3) . .
C23 C18 P2 124.7(2) . .
C19 C18 P2 117.3(2) . .
C20 C19 C18 120.8(3) . .
C20 C19 H19 119.6 . .
C18 C19 H19 119.6 . .
C21 C20 C19 119.8(4) . .
C21 C20 H20 120.1 . .
C19 C20 H20 120.1 . .
C22 C21 C20 120.0(4) . .
C22 C21 H21 120.0 . .
C20 C21 H21 120.0 . .
C21 C22 C23 120.8(4) . .
C21 C22 H22 119.6 . .
C23 C22 H22 119.6 . .
C18 C23 C22 120.5(4) . .
C18 C23 H23 119.8 . .
C22 C23 H23 119.8 . .
C25 C24 C29 119.1(2) . .
C25 C24 P2 123.6(2) . .
C29 C24 P2 117.2(2) . .
C24 C25 C26 120.0(3) . .
C24 C25 H25 120.0 . .
C26 C25 H25 120.0 . .
C27 C26 C25 120.5(3) . .
C27 C26 H26 119.8 . .
C25 C26 H26 119.8 . .
C26 C27 C28 120.4(3) . .
C26 C27 H27 119.8 . .
C28 C27 H27 119.8 . .
C27 C28 C29 119.8(3) . .
C27 C28 H28 120.1 . .
C29 C28 H28 120.1 . .
C28 C29 C24 120.2(3) . .
C28 C29 H29 119.9 . .
C24 C29 H29 119.9 . .
O1 C30 H30A 109.5 . .
O1 C30 H30B 109.5 . .
H30A C30 H30B 109.5 . .
O1 C30 H30C 109.5 . .
H30A C30 H30C 109.5 . .
H30B C30 H30C 109.5 . .
C30 O1 H1O1 104.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 P1 2.4633(11) .
Ag1 P2 2.4634(10) 2_666
Ag1 Cl1 2.6660(11) .
Ag1 Cl1 2.6807(9) 2_666
P1 C12 1.824(2) .
P1 C6 1.830(3) .
P1 C1 1.841(3) .
P2 C18 1.813(3) .
P2 C24 1.827(2) .
P2 C5 1.850(2) .
P2 Ag1 2.4634(10) 2_666
Cl1 Ag1 2.6807(9) 2_666
N1 C1 1.470(3) .
N1 C2 1.478(3) .
N1 C4 1.484(3) .
N2 C5 1.444(3) .
N2 C4 1.470(3) .
N2 C3 1.481(3) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C2 C3 1.509(4) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C6 C11 1.385(3) .
C6 C7 1.389(3) .
C7 C8 1.378(4) .
C7 H7 0.9400 .
C8 C9 1.375(4) .
C8 H8 0.9400 .
C9 C10 1.380(4) .
C9 H9 0.9400 .
C10 C11 1.381(4) .
C10 H10 0.9400 .
C11 H11 0.9400 .
C12 C13 1.386(4) .
C12 C17 1.395(3) .
C13 C14 1.389(4) .
C13 H13 0.9400 .
C14 C15 1.390(4) .
C14 H14 0.9400 .
C15 C16 1.364(4) .
C15 H15 0.9400 .
C16 C17 1.391(4) .
C16 H16 0.9400 .
C17 H17 0.9400 .
C18 C23 1.368(4) .
C18 C19 1.392(4) .
C19 C20 1.390(5) .
C19 H19 0.9400 .
C20 C21 1.368(6) .
C20 H20 0.9400 .
C21 C22 1.347(6) .
C21 H21 0.9400 .
C22 C23 1.398(5) .
C22 H22 0.9400 .
C23 H23 0.9400 .
C24 C25 1.388(4) .
C24 C29 1.399(4) .
C25 C26 1.391(4) .
C25 H25 0.9400 .
C26 C27 1.371(5) .
C26 H26 0.9400 .
C27 C28 1.379(5) .
C27 H27 0.9400 .
C28 C29 1.391(4) .
C28 H28 0.9400 .
C29 H29 0.9400 .
C30 O1 1.414(5) .
C30 H30A 0.9700 .
C30 H30B 0.9700 .
C30 H30C 0.9700 .
O1 H1O1 0.8500 .
