#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/28/2212807.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2212807
loop_
_publ_author_name
'Li, Yu-Feng'
'Wu, Hui'
'Li, Yi-Zhi'
'Zhang, Hong'
'Pan, Yi'
_publ_section_title
Bis(μ-3-methylbut-2-enoato-κ²O:O)bis{[(2-methoxyphenyl)diphenylphosphine-κP]silver(I)}
_journal_coeditor_code           CF2093
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1068
_journal_page_last               m1069
_journal_paper_doi               10.1107/S1600536807011531
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Ag2 (C5 H12 O2)2 (C19 H17 O P)2]'
_chemical_formula_moiety         'C48 H48 Ag2 O6 P2'
_chemical_formula_sum            'C48 H48 Ag2 O6 P2'
_chemical_formula_weight         998.54
_chemical_name_systematic
;
Bis(μ₂-(3-methylbut-2-enoato-κ²O:O)bis{[(2-
methoxyphenyl)diphenylphosphine-\kP]silver(I)}
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 105.09(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.6740(17)
_cell_length_b                   16.500(3)
_cell_length_c                   16.365(3)
_cell_measurement_reflns_used    784
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      25.77
_cell_measurement_theta_min      2.33
_cell_volume                     2261.4(8)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0605
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9168
_diffrn_reflns_theta_full        26.0
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.78
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.983
_exptl_absorpt_correction_T_max  0.787
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.319
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         4441
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.04P)²+1.22P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1013
_reflns_number_gt                3125
_reflns_number_total             4441
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cf2093.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2212807
_cod_database_fobs_code          2212807
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Ag Ag1 0.67385(4) -0.00340(2) 0.08966(2) 0.03431(11) Uani d . 1
C C1 0.2319(6) 0.3331(3) -0.0269(3) 0.0494(13) Uani d . 1
H H1A 0.1506 0.2960 -0.0558 0.074 Uiso calc R 1
H H1B 0.2496 0.3731 -0.0660 0.074 Uiso calc R 1
H H1C 0.1981 0.3594 0.0179 0.074 Uiso calc R 1
C C2 0.4974(7) 0.3349(3) 0.0714(4) 0.0522(13) Uani d . 1
H H2A 0.4664 0.3359 0.1236 0.078 Uiso calc R 1
H H2B 0.5000 0.3893 0.0509 0.078 Uiso calc R 1
H H2C 0.6015 0.3110 0.0808 0.078 Uiso calc R 1
C C3 0.3835(6) 0.2877(3) 0.0096(3) 0.0503(13) Uani d . 1
C C4 0.4003(6) 0.2132(3) -0.0104(3) 0.0465(12) Uani d . 1
H H4A 0.3164 0.1916 -0.0522 0.056 Uiso calc R 1
C C5 0.5350(6) 0.1575(3) 0.0243(3) 0.0415(11) Uani d . 1
C C6 1.0560(7) -0.1147(4) 0.0247(4) 0.0544(14) Uani d . 1
H H6A 1.0622 -0.0713 -0.0134 0.082 Uiso calc R 1
H H6B 0.9808 -0.1545 -0.0044 0.082 Uiso calc R 1
H H6C 1.1593 -0.1394 0.0447 0.082 Uiso calc R 1
C C11 1.0668(5) -0.0144(3) 0.2210(3) 0.0426(11) Uani d U 1
C C12 1.1733(7) 0.0260(3) 0.2856(3) 0.0485(13) Uani d . 1
H H12A 1.1379 0.0460 0.3306 0.058 Uiso calc R 1
C C13 1.3286(7) 0.0374(4) 0.2853(3) 0.0539(14) Uani d . 1
H H13A 1.3986 0.0645 0.3296 0.065 Uiso calc R 1
C C14 1.3804(6) 0.0077(3) 0.2175(3) 0.0438(11) Uani d . 1
H H14A 1.4862 0.0155 0.2166 0.053 Uiso calc R 1
C C15 1.2805(6) -0.0323(3) 0.1525(4) 0.0522(13) Uani d . 1
H H15A 1.3169 -0.0509 0.1072 0.063 Uiso calc R 1
C C16 1.1216(6) -0.0454(3) 0.1544(3) 0.0424(11) Uani d U 1
C C21 0.8523(6) -0.1282(3) 0.2610(3) 0.0428(11) Uani d . 1
C C22 0.9867(6) -0.1682(3) 0.3111(3) 0.0430(11) Uani d . 1
H H22A 1.0849 -0.1420 0.3259 0.052 Uiso calc R 1
C C23 0.9734(7) -0.2461(3) 0.3383(3) 0.0534(14) Uani d . 1
H H23A 1.0652 -0.2731 0.3676 0.064 Uiso calc R 1
C C24 0.8289(7) -0.2853(3) 0.3235(3) 0.0489(13) Uani d . 1
H H24A 0.8208 -0.3361 0.3467 0.059 Uiso calc R 1
C C25 0.6925(5) -0.2461(3) 0.2720(3) 0.0403(11) Uani d . 1
H H25A 0.5945 -0.2726 0.2580 0.048 Uiso calc R 1
C C26 0.7051(6) -0.1699(3) 0.2430(3) 0.0421(11) Uani d . 1
H H26A 0.6142 -0.1444 0.2104 0.050 Uiso calc R 1
C C31 0.8260(6) 0.0412(3) 0.3021(3) 0.0467(12) Uani d . 1
C C32 0.7912(6) 0.1214(3) 0.2811(3) 0.0416(10) Uani d U 1
H H32A 0.7863 0.1392 0.2265 0.050 Uiso calc R 1
C C33 0.7642(7) 0.1745(4) 0.3390(3) 0.0547(13) Uani d U 1
H H33A 0.7420 0.2283 0.3234 0.066 Uiso calc R 1
C C34 0.7687(6) 0.1510(3) 0.4211(3) 0.0438(12) Uani d . 1
H H34A 0.7485 0.1876 0.4603 0.053 Uiso calc R 1
C C35 0.8033(6) 0.0732(4) 0.4414(4) 0.0502(12) Uani d U 1
H H35A 0.8094 0.0564 0.4964 0.060 Uiso calc R 1
C C36 0.8304(6) 0.0167(3) 0.3838(3) 0.0497(12) Uani d U 1
H H36A 0.8514 -0.0371 0.3998 0.060 Uiso calc R 1
O O1 0.5167(4) 0.0831(2) 0.0051(2) 0.0434(8) Uani d . 1
O O2 0.6664(4) 0.1828(2) 0.0661(2) 0.0507(9) Uani d . 1
O O3 1.0064(4) -0.0841(2) 0.0935(2) 0.0455(8) Uani d . 1
P P1 0.85814(14) -0.02802(7) 0.21982(7) 0.0345(3) Uani d . 1
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'
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'
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_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Ag1 P1 . 148.23(9) y
O1 Ag1 O1 3_655 74.54(13) y
P1 Ag1 O1 3_655 134.34(9) y
C3 C1 H1A . 109.5 ?
C3 C1 H1B . 109.5 ?
H1A C1 H1B . 109.5 ?
C3 C1 H1C . 109.5 ?
H1A C1 H1C . 109.5 ?
H1B C1 H1C . 109.5 ?
C3 C2 H2A . 109.5 ?
C3 C2 H2B . 109.5 ?
H2A C2 H2B . 109.5 ?
C3 C2 H2C . 109.5 ?
H2A C2 H2C . 109.5 ?
H2B C2 H2C . 109.5 ?
C4 C3 C2 . 126.2(5) ?
C4 C3 C1 . 121.5(5) ?
C2 C3 C1 . 112.2(5) ?
C3 C4 C5 . 128.7(5) ?
C3 C4 H4A . 115.7 ?
C5 C4 H4A . 115.7 ?
O2 C5 O1 . 120.1(4) ?
O2 C5 C4 . 121.6(5) ?
O1 C5 C4 . 118.1(4) ?
O3 C6 H6A . 109.5 ?
O3 C6 H6B . 109.5 ?
H6A C6 H6B . 109.5 ?
O3 C6 H6C . 109.5 ?
H6A C6 H6C . 109.5 ?
H6B C6 H6C . 109.5 ?
C12 C11 C16 . 118.6(5) ?
C12 C11 P1 . 122.3(4) ?
C16 C11 P1 . 119.1(4) ?
C13 C12 C11 . 122.0(5) ?
C13 C12 H12A . 119.0 ?
C11 C12 H12A . 119.0 ?
C12 C13 C14 . 118.6(5) ?
C12 C13 H13A . 120.7 ?
C14 C13 H13A . 120.7 ?
C15 C14 C13 . 121.6(5) ?
C15 C14 H14A . 119.2 ?
C13 C14 H14A . 119.2 ?
C14 C15 C16 . 119.2(5) ?
C14 C15 H15A . 120.4 ?
C16 C15 H15A . 120.4 ?
O3 C16 C11 . 114.0(4) ?
O3 C16 C15 . 126.1(5) ?
C11 C16 C15 . 119.9(5) ?
C22 C21 C26 . 117.4(5) ?
C22 C21 P1 . 123.6(4) ?
C26 C21 P1 . 118.9(4) ?
C23 C22 C21 . 120.1(5) ?
C23 C22 H22A . 119.9 ?
C21 C22 H22A . 119.9 ?
C22 C23 C24 . 122.2(5) ?
C22 C23 H23A . 118.9 ?
C24 C23 H23A . 118.9 ?
C23 C24 C25 . 118.1(5) ?
C23 C24 H24A . 121.0 ?
C25 C24 H24A . 121.0 ?
C26 C25 C24 . 120.0(5) ?
C26 C25 H25A . 120.0 ?
C24 C25 H25A . 120.0 ?
C25 C26 C21 . 121.9(5) ?
C25 C26 H26A . 119.0 ?
C21 C26 H26A . 119.0 ?
C32 C31 C36 . 118.0(5) ?
C32 C31 P1 . 118.5(4) ?
C36 C31 P1 . 123.5(4) ?
C33 C32 C31 . 120.8(5) ?
C33 C32 H32A . 119.6 ?
C31 C32 H32A . 119.6 ?
C32 C33 C34 . 121.9(5) ?
C32 C33 H33A . 119.0 ?
C34 C33 H33A . 119.0 ?
C35 C34 C33 . 117.1(5) ?
C35 C34 H34A . 121.4 ?
C33 C34 H34A . 121.4 ?
C34 C35 C36 . 122.7(5) ?
C34 C35 H35A . 118.6 ?
C36 C35 H35A . 118.6 ?
C31 C36 C35 . 119.4(5) ?
C31 C36 H36A . 120.3 ?
C35 C36 H36A . 120.3 ?
C5 O1 Ag1 . 117.1(3) y
C5 O1 Ag1 3_655 136.6(3) y
Ag1 O1 Ag1 3_655 105.46(13) y
C16 O3 C6 . 115.7(4) y
C21 P1 C11 . 103.6(2) y
C21 P1 C31 . 105.9(2) y
C11 P1 C31 . 104.8(2) y
C21 P1 Ag1 . 115.02(17) y
C11 P1 Ag1 . 115.46(17) y
C31 P1 Ag1 . 111.10(17) y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ag1 O1 . 2.197(3) y
Ag1 P1 . 2.3420(14) y
Ag1 O1 3_655 2.352(3) y
C1 C3 . 1.496(7) ?
C1 H1A . 0.960 ?
C1 H1B . 0.960 ?
C1 H1C . 0.960 ?
C2 C3 . 1.445(7) ?
C2 H2A . 0.960 ?
C2 H2B . 0.960 ?
C2 H2C . 0.960 ?
C3 C4 . 1.289(7) ?
C4 C5 . 1.479(7) ?
C4 H4A . 0.930 ?
C5 O2 . 1.239(6) ?
C5 O1 . 1.267(6) ?
C6 O3 . 1.400(6) ?
C6 H6A . 0.960 ?
C6 H6B . 0.960 ?
C6 H6C . 0.960 ?
C11 C12 . 1.380(7) ?
C11 C16 . 1.394(7) ?
C11 P1 . 1.819(5) ?
C12 C13 . 1.362(8) ?
C12 H12A . 0.930 ?
C13 C14 . 1.391(8) ?
C13 H13A . 0.930 ?
C14 C15 . 1.355(8) ?
C14 H14A . 0.930 ?
C15 C16 . 1.404(7) ?
C15 H15A . 0.930 ?
C16 O3 . 1.372(6) y
C21 C22 . 1.403(7) ?
C21 C26 . 1.412(7) ?
C21 P1 . 1.790(5) ?
C22 C23 . 1.374(7) ?
C22 H22A . 0.930 ?
C23 C24 . 1.375(8) ?
C23 H23A . 0.930 ?
C24 C25 . 1.417(7) ?
C24 H24A . 0.930 ?
C25 C26 . 1.359(7) ?
C25 H25A . 0.930 ?
C26 H26A . 0.930 ?
C31 C32 . 1.380(8) ?
C31 C36 . 1.387(8) ?
C31 P1 . 1.842(5) ?
C32 C33 . 1.356(7) ?
C32 H32A . 0.930 ?
C33 C34 . 1.389(7) ?
C33 H33A . 0.930 ?
C34 C35 . 1.339(8) ?
C34 H34A . 0.930 ?
C35 C36 . 1.389(7) ?
C35 H35A . 0.930 ?
C36 H36A . 0.930 ?
O1 Ag1 3_655 2.352(3) ?
