#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:31:04 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179144 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/05/4310598.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_4310598
loop_
_publ_author_name
'Eric Fournier'
'Stéphanie Sicard'
'Andreas Decken'
'Pierre D. Harvey'
_publ_section_title
;
 Organometallic Oligomers Based on 1,8-Diisocyano-p-menthane (dmb):
 Syntheses and Characterization of the {[M(diphos)(dmb)]BF4}n and
 {[Pd2(diphos)2(dmb)](ClO4)2}n Materials (M = Cu, Ag; diphos = dppe, dppp)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1491
_journal_page_last               1501
_journal_paper_doi               10.1021/ic034780z
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C54 H52 Ag2 B2 F8 P4'
_chemical_formula_weight         1214.20
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.9480(10)
_cell_angle_beta                 114.1240(10)
_cell_angle_gamma                112.6470(10)
_cell_formula_units_Z            1
_cell_length_a                   10.6110(6)
_cell_length_b                   11.3248(7)
_cell_length_c                   12.8341(7)
_cell_measurement_temperature    173(2)
_cell_volume                     1271.02(13)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_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  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9111
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.963
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepip
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.575
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         5652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0258
_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)+(0.0426P)²+0.4137P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0681
_refine_ls_wR_factor_ref         0.0689
_reflns_number_gt                5360
_reflns_number_total             5652
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034780zsi20031215_104820.cif
_cod_data_source_block           ph
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4310598
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag Ag 0.898817(12) 0.385928(12) 0.299285(11) 0.02868(6) Uani 1 1 d . . .
P1 P 0.64615(4) 0.26036(4) 0.27662(3) 0.02306(9) Uani 1 1 d . . .
P2 P 1.13944(5) 0.43419(4) 0.30231(4) 0.02406(9) Uani 1 1 d . . .
C1 C 0.59108(19) 0.34367(17) 0.36094(15) 0.0272(3) Uani 1 1 d . . .
C2 C 0.70423(19) 0.38201(17) 0.49018(14) 0.0268(3) Uani 1 1 d . . .
C3 C 0.69968(19) 0.49431(18) 0.55252(15) 0.0299(3) Uani 1 1 d . . .
C4 C 0.6205(2) 0.10685(16) 0.32203(14) 0.0287(3) Uani 1 1 d . . .
C5 C 0.4899(3) 0.0304(2) 0.3317(2) 0.0447(5) Uani 1 1 d . . .
C6 C 0.4729(3) -0.0873(2) 0.3668(2) 0.0610(7) Uani 1 1 d . . .
C7 C 0.5858(4) -0.1282(2) 0.3922(2) 0.0616(7) Uani 1 1 d . . .
C8 C 0.7152(4) -0.0540(3) 0.3830(2) 0.0567(6) Uani 1 1 d . . .
C9 C 0.7338(3) 0.0644(2) 0.34840(18) 0.0404(4) Uani 1 1 d . . .
C10 C 0.49633(18) 0.22072(17) 0.12892(14) 0.0272(3) Uani 1 1 d . . .
C11 C 0.4584(2) 0.3189(2) 0.08269(16) 0.0333(4) Uani 1 1 d . . .
C12 C 0.3466(2) 0.2922(2) -0.03083(18) 0.0415(4) Uani 1 1 d . . .
C13 C 0.2755(2) 0.1697(3) -0.09897(17) 0.0457(5) Uani 1 1 d . . .
C14 C 0.3138(3) 0.0725(2) -0.05463(18) 0.0452(5) Uani 1 1 d . . .
C15 C 0.4240(2) 0.0968(2) 0.05945(16) 0.0350(4) Uani 1 1 d . . .
C16 C 1.1949(2) 0.54000(17) 0.21059(16) 0.0334(4) Uani 1 1 d . . .
C17 C 1.1078(3) 0.6028(2) 0.15133(18) 0.0454(5) Uani 1 1 d . . .
C18 C 1.1552(5) 0.6866(3) 0.0823(2) 0.0742(10) Uani 1 1 d . . .
C19 C 1.2845(5) 0.7043(3) 0.0736(3) 0.0877(14) Uani 1 1 d . . .
C20 C 1.3711(5) 0.6432(3) 0.1331(4) 0.0814(12) Uani 1 1 d . . .
C21 C 1.3291(3) 0.5630(2) 0.2022(3) 0.0532(6) Uani 1 1 d . . .
C22 C 1.14295(18) 0.28120(17) 0.26291(15) 0.0276(3) Uani 1 1 d . . .
C23 C 1.1475(2) 0.24627(19) 0.16113(17) 0.0326(4) Uani 1 1 d . . .
C24 C 1.1361(2) 0.1225(2) 0.13166(19) 0.0401(4) Uani 1 1 d . . .
C25 C 1.1199(2) 0.0352(2) 0.2027(2) 0.0427(5) Uani 1 1 d . . .
C26 C 1.1170(2) 0.0695(2) 0.30503(19) 0.0409(4) Uani 1 1 d . . .
C27 C 1.1282(2) 0.19179(19) 0.33475(17) 0.0347(4) Uani 1 1 d . . .
B B 0.8816(3) 0.6725(2) 0.3529(2) 0.0451(5) Uani 1 1 d . . .
F1 F 0.94579(16) 0.61408(13) 0.44186(12) 0.0516(3) Uani 1 1 d . . .
F2 F 0.7394(3) 0.6602(3) 0.3468(3) 0.0855(9) Uani 0.75 1 d P . .
F3 F 0.8358(5) 0.5959(4) 0.2520(3) 0.0919(15) Uani 0.75 1 d P . .
F4 F 0.9629(4) 0.7952(3) 0.3642(4) 0.1218(17) Uani 0.75 1 d P . .
F2A F 1.0246(13) 0.7457(9) 0.3314(9) 0.097(3) Uani 0.25 1 d P . .
F3A F 0.873(2) 0.7601(13) 0.3977(9) 0.116(5) Uani 0.25 1 d P . .
F4A F 0.7922(13) 0.5898(8) 0.2562(10) 0.124(7) Uani 0.25 1 d P . .
H1A H 0.488(2) 0.284(2) 0.3499(18) 0.025(5) Uiso 1 1 d . . .
H2A H 0.683(3) 0.308(2) 0.528(2) 0.036(6) Uiso 1 1 d . . .
H3A H 0.606(3) 0.465(2) 0.5610(19) 0.033(5) Uiso 1 1 d . . .
H1B H 0.592(3) 0.416(2) 0.3292(19) 0.033(5) Uiso 1 1 d . . .
H2B H 0.804(3) 0.407(2) 0.4998(18) 0.029(5) Uiso 1 1 d . . .
H3B H 0.709(3) 0.564(2) 0.513(2) 0.034(6) Uiso 1 1 d . . .
H5 H 0.420(3) 0.060(3) 0.320(2) 0.057(8) Uiso 1 1 d . . .
H6 H 0.389(4) -0.128(3) 0.377(3) 0.070(9) Uiso 1 1 d . . .
H7 H 0.572(4) -0.208(4) 0.415(3) 0.094(12) Uiso 1 1 d . . .
H8 H 0.783(4) -0.081(3) 0.396(3) 0.072(10) Uiso 1 1 d . . .
H9 H 0.826(3) 0.119(3) 0.349(2) 0.047(7) Uiso 1 1 d . . .
H11 H 0.506(3) 0.400(2) 0.126(2) 0.038(6) Uiso 1 1 d . . .
H12 H 0.320(3) 0.353(3) -0.059(2) 0.050(7) Uiso 1 1 d . . .
H13 H 0.212(3) 0.159(3) -0.172(2) 0.053(7) Uiso 1 1 d . . .
H14 H 0.273(3) -0.011(3) -0.098(2) 0.052(7) Uiso 1 1 d . . .
H15 H 0.451(3) 0.032(3) 0.093(2) 0.046(7) Uiso 1 1 d . . .
H17 H 1.035(3) 0.593(2) 0.1623(18) 0.024(5) Uiso 1 1 d . . .
H18 H 1.097(4) 0.718(4) 0.054(3) 0.075(11) Uiso 1 1 d . . .
H19 H 1.312(5) 0.751(4) 0.033(4) 0.111(14) Uiso 1 1 d . . .
H20 H 1.464(5) 0.664(4) 0.128(3) 0.098(12) Uiso 1 1 d . . .
H21 H 1.381(5) 0.511(4) 0.237(4) 0.106(14) Uiso 1 1 d . . .
H23 H 1.160(3) 0.307(2) 0.113(2) 0.033(5) Uiso 1 1 d . . .
H24 H 1.131(3) 0.100(2) 0.055(2) 0.039(6) Uiso 1 1 d . . .
H25 H 1.114(3) -0.047(3) 0.184(2) 0.055(7) Uiso 1 1 d . . .
H26 H 1.106(3) 0.012(3) 0.355(2) 0.054(7) Uiso 1 1 d . . .
H27 H 1.120(3) 0.210(2) 0.400(2) 0.041(6) Uiso 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'
B B 0.0013 0.0007 '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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P2 Ag P1 159.409(16) . . ?
C4 P1 C10 105.77(8) . . ?
C4 P1 C1 105.26(8) . . ?
C10 P1 C1 103.71(8) . . ?
C4 P1 Ag 113.30(6) . . ?
C10 P1 Ag 114.65(5) . . ?
C1 P1 Ag 113.18(6) . . ?
C16 P2 C22 107.24(8) . . ?
C16 P2 C3 104.79(9) . 2_766 ?
C22 P2 C3 103.44(8) . 2_766 ?
C16 P2 Ag 118.43(7) . . ?
C22 P2 Ag 108.31(5) . . ?
C3 P2 Ag 113.48(6) 2_766 . ?
C2 C1 P1 111.02(11) . . ?
C3 C2 C1 111.28(14) . . ?
C2 C3 P2 112.18(12) . 2_766 ?
C5 C4 C9 119.08(19) . . ?
C5 C4 P1 121.36(15) . . ?
C9 C4 P1 119.56(15) . . ?
C4 C5 C6 120.3(2) . . ?
C7 C6 C5 119.9(3) . . ?
C8 C7 C6 120.5(2) . . ?
C7 C8 C9 120.1(2) . . ?
C4 C9 C8 120.1(2) . . ?
C15 C10 C11 119.31(17) . . ?
C15 C10 P1 121.83(14) . . ?
C11 C10 P1 118.79(14) . . ?
C12 C11 C10 120.1(2) . . ?
C13 C12 C11 120.3(2) . . ?
C12 C13 C14 120.03(19) . . ?
C13 C14 C15 120.5(2) . . ?
C10 C15 C14 119.7(2) . . ?
C17 C16 C21 119.4(2) . . ?
C17 C16 P2 119.99(16) . . ?
C21 C16 P2 120.61(18) . . ?
C16 C17 C18 118.8(3) . . ?
C19 C18 C17 120.3(3) . . ?
C20 C19 C18 120.7(3) . . ?
C19 C20 C21 120.2(3) . . ?
C20 C21 C16 120.6(3) . . ?
C23 C22 C27 119.11(17) . . ?
C23 C22 P2 123.19(14) . . ?
C27 C22 P2 117.50(13) . . ?
C22 C23 C24 119.92(19) . . ?
C25 C24 C23 120.26(19) . . ?
C24 C25 C26 120.32(19) . . ?
C27 C26 C25 119.8(2) . . ?
C26 C27 C22 120.64(19) . . ?
F3A B F4A 132.1(10) . . ?
F3A B F4 54.8(7) . . ?
F4A B F4 125.5(5) . . ?
F3A B F3 145.3(6) . . ?
F4A B F3 20.4(8) . . ?
F4 B F3 115.7(4) . . ?
F3A B F1 106.6(4) . . ?
F4A B F1 111.3(5) . . ?
F4 B F1 115.7(2) . . ?
F3 B F1 106.9(2) . . ?
F3A B F2 58.7(8) . . ?
F4A B F2 81.7(8) . . ?
F4 B F2 106.9(3) . . ?
F3 B F2 101.9(3) . . ?
F1 B F2 108.9(2) . . ?
F3A B F2A 102.4(8) . . ?
F4A B F2A 100.0(8) . . ?
F4 B F2A 48.2(4) . . ?
F3 B F2A 81.1(5) . . ?
F1 B F2A 98.2(4) . . ?
F2 B F2A 150.3(4) . . ?
F3A F2 B 51.5(3) . . ?
F3A F2 F4A 93.2(4) . . ?
B F2 F4A 45.4(3) . . ?
F3A F4 F2A 135.4(6) . . ?
F3A F4 B 58.3(5) . . ?
F2A F4 B 78.0(5) . . ?
F4 F2A B 53.8(4) . . ?
F4 F3A B 66.9(5) . . ?
F4 F3A F2 126.5(8) . . ?
B F3A F2 69.8(7) . . ?
B F4A F2 52.9(6) . . ?
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
Ag P2 2.3797(4) . ?
Ag P1 2.3890(4) . ?
P1 C4 1.7986(17) . ?
P1 C10 1.8114(17) . ?
P1 C1 1.8195(17) . ?
P2 C16 1.7993(19) . ?
P2 C22 1.8153(17) . ?
P2 C3 1.8239(18) 2_766 ?
C1 C2 1.526(2) . ?
C2 C3 1.518(2) . ?
C3 P2 1.8239(17) 2_766 ?
C4 C5 1.381(3) . ?
C4 C9 1.381(3) . ?
C5 C6 1.383(3) . ?
C6 C7 1.367(5) . ?
C7 C8 1.361(5) . ?
C8 C9 1.386(3) . ?
C10 C15 1.386(3) . ?
C10 C11 1.387(3) . ?
C11 C12 1.385(3) . ?
C12 C13 1.369(3) . ?
C13 C14 1.370(4) . ?
C14 C15 1.388(3) . ?
C16 C17 1.374(3) . ?
C16 C21 1.396(3) . ?
C17 C18 1.402(4) . ?
C18 C19 1.360(6) . ?
C19 C20 1.356(6) . ?
C20 C21 1.359(4) . ?
C22 C23 1.384(2) . ?
C22 C27 1.388(3) . ?
C23 C24 1.391(3) . ?
C24 C25 1.366(3) . ?
C25 C26 1.379(3) . ?
C26 C27 1.377(3) . ?
B F3A 1.193(7) . ?
B F4A 1.278(11) . ?
B F4 1.290(3) . ?
B F3 1.337(4) . ?
B F1 1.394(3) . ?
B F2 1.430(4) . ?
B F2A 1.564(9) . ?
F2 F3A 1.302(17) . ?
F2 F4A 1.775(18) . ?
F4 F3A 1.145(12) . ?
F4 F2A 1.192(9) . ?
