#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:08:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180027 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/21/7032172.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_7032172
loop_
_publ_author_name
'Edwards, Peter G.'
'Kariuki, Benson M.'
'Newman, Paul D.'
'Tallis, Huw A.'
'Williams, Craig'
_publ_section_title
;
 Aspects of the coordination chemistry of
 rac-trans-1,2-diphosphinocyclohexane and the preparation of reinforced
 9aneP3 and 9anePN2 macrocycles.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15532
_journal_page_last               15545
_journal_paper_doi               10.1039/c4dt02239d
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C30 H50 Ag3 P10, 3(C F3 O3 S)'
_chemical_formula_sum            'C33 H50 Ag3 F9 O9 P10 S3'
_chemical_formula_weight         1491.22
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 99.030(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8754(3)
_cell_length_b                   23.0437(9)
_cell_length_c                   13.1527(3)
_cell_measurement_reflns_used    4542
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.242
_cell_measurement_theta_min      2.088
_cell_volume                     2956.01(16)
_computing_cell_refinement       DENZO/SCALEPACK
_computing_data_collection       'cOLLECT,Nonius BV, 1997-2001'
_computing_data_reduction        DENZO/SCALEPACK
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SHELXs-97
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0626
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11498
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.463
_diffrn_reflns_theta_min         2.088
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.430
_exptl_absorpt_correction_T_max  0.8702
_exptl_absorpt_correction_T_min  0.6735
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Denzo/Scalepack
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_description       needle
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.068
_refine_diff_density_min         -1.045
_refine_diff_density_rms         0.142
_refine_ls_extinction_coef       0.0094(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6912
_refine_ls_number_restraints     638
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0749
_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)+(0.1027P)²+12.2417P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1911
_refine_ls_wR_factor_ref         0.2190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4542
_reflns_number_total             6912
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4dt02239d1.cif
_cod_data_source_block           shelx_cmpd2
_cod_depositor_comments
'Adding full bibliography for 7032169--7032173.cif.'
_cod_database_code               7032172
#BEGIN Tags that were not found in dictionaries:
_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   0.674
_shelx_estimated_absorpt_t_max   0.870
_shelxl_version_number           2013-4
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8745(6) 0.3714(3) 0.1673(5) 0.0384(14) Uani 1 1 d . . . . .
H1 H 0.8481 0.3304 0.1492 0.046 Uiso 1 1 calc R U . . .
C2 C 0.8068(7) 0.3883(3) 0.2601(5) 0.0462(16) Uani 1 1 d . . . . .
H2A H 0.8284 0.4293 0.2783 0.055 Uiso 1 1 calc R U . . .
H2B H 0.7060 0.3848 0.2416 0.055 Uiso 1 1 calc R U . . .
C3 C 0.8562(9) 0.3499(4) 0.3527(5) 0.0565(19) Uani 1 1 d . . . . .
H3A H 0.8294 0.3092 0.3363 0.068 Uiso 1 1 calc R U . . .
H3B H 0.8123 0.3624 0.4118 0.068 Uiso 1 1 calc R U . . .
C4 C 1.0115(9) 0.3538(4) 0.3817(6) 0.058(2) Uani 1 1 d . . . . .
H4A H 1.0374 0.3939 0.4037 0.069 Uiso 1 1 calc R U . . .
H4B H 1.0422 0.3276 0.4403 0.069 Uiso 1 1 calc R U . . .
C5 C 1.0829(9) 0.3373(4) 0.2917(6) 0.060(2) Uani 1 1 d . . . . .
H5A H 1.0667 0.2957 0.2758 0.071 Uiso 1 1 calc R U . . .
H5B H 1.1829 0.3431 0.3114 0.071 Uiso 1 1 calc R U . . .
C6 C 1.0319(7) 0.3734(3) 0.1950(5) 0.0425(15) Uani 1 1 d . . . . .
H6 H 1.0612 0.4146 0.2081 0.051 Uiso 1 1 calc R U . . .
C7 C 0.7856(10) 0.2686(6) -0.2127(9) 0.052(4) Uani 0.5 1 d D . P . .
H7 H 0.7856 0.3119 -0.2150 0.063 Uiso 0.5 1 calc R U P . .
C8 C 0.9154(12) 0.2500 -0.2545(7) 0.100(6) Uani 1 2 d DS T P . .
H8 H 0.8995 0.2074 -0.2486 0.120 Uiso 0.5 1 calc R U P . .
C9 C 0.9090(14) 0.2500 -0.3719(7) 0.074(4) Uani 1 2 d DS T P . .
H9A H 0.9808 0.2234 -0.3889 0.089 Uiso 0.5 1 calc R U P . .
H9B H 0.9327 0.2895 -0.3931 0.089 Uiso 0.5 1 calc R U P . .
C10 C 0.7721(15) 0.2325(9) -0.4371(12) 0.095(9) Uani 0.5 1 d D . P . .
H10A H 0.7696 0.2493 -0.5067 0.114 Uiso 1 2 calc R U P . .
H10B H 0.7718 0.1898 -0.4448 0.114 Uiso 0.5 1 calc R U P . .
C11 C 0.639(2) 0.2500 -0.3983(8) 0.155(9) Uani 1 2 d DS TU P . .
H11A H 0.5656 0.2229 -0.4272 0.186 Uiso 0.5 1 calc R U P . .
H11B H 0.6125 0.2893 -0.4243 0.186 Uiso 0.5 1 calc R U P . .
C12 C 0.6514(12) 0.2500 -0.2804(8) 0.072(4) Uani 1 2 d DS T P . .
H12A H 0.6303 0.2102 -0.2594 0.087 Uiso 0.5 1 calc R U P . .
H12B H 0.5779 0.2755 -0.2626 0.087 Uiso 0.5 1 calc R U P . .
C13 C 0.5903(9) 0.5359(4) 0.2755(6) 0.069(2) Uani 1 1 d . . . . .
H13 H 0.6882 0.5259 0.2726 0.083 Uiso 1 1 calc R U . . .
C14 C 0.5678(9) 0.5983(4) 0.2402(7) 0.071(2) Uani 1 1 d . . . . .
H14 H 0.4699 0.6080 0.2437 0.085 Uiso 1 1 calc R U . . .
C15 C 0.6543(9) 0.6377(5) 0.3135(8) 0.083(3) Uani 1 1 d . . . . .
H15A H 0.6349 0.6783 0.2912 0.100 Uiso 1 1 calc R U . . .
H15B H 0.7519 0.6299 0.3095 0.100 Uiso 1 1 calc R U . . .
C16 C 0.6331(14) 0.6319(6) 0.4254(9) 0.107(4) Uani 1 1 d . . . . .
H16A H 0.6979 0.6576 0.4695 0.128 Uiso 1 1 calc R U . . .
H16B H 0.5386 0.6438 0.4323 0.128 Uiso 1 1 calc R U . . .
C17 C 0.6565(15) 0.5702(6) 0.4587(9) 0.102(4) Uani 1 1 d . . . . .
H17A H 0.6358 0.5658 0.5295 0.122 Uiso 1 1 calc R U . . .
H17B H 0.7542 0.5603 0.4597 0.122 Uiso 1 1 calc R U . . .
C18 C 0.5669(11) 0.5283(5) 0.3870(7) 0.081(3) Uani 1 1 d . . . . .
H18A H 0.5889 0.4879 0.4093 0.097 Uiso 1 1 calc R U . . .
H18B H 0.4692 0.5354 0.3915 0.097 Uiso 1 1 calc R U . . .
Ag1 Ag 1.04195(8) 0.2500 0.00814(6) 0.0501(3) Uani 1 2 d S T P . .
Ag2 Ag 0.55636(6) 0.43717(3) 0.03818(5) 0.0645(3) Uani 1 1 d . . . . .
P1 P 0.80393(18) 0.41715(9) 0.05644(14) 0.0456(5) Uani 1 1 d . . . . .
P2 P 1.11561(19) 0.34417(9) 0.08925(15) 0.0478(5) Uani 1 1 d . . . . .
P3 P 1.0777(3) 0.2500 -0.1779(2) 0.0529(7) Uani 1 2 d S T P . .
P4 P 0.7911(3) 0.2500 -0.0777(2) 0.0507(7) Uani 1 2 d S T P . .
P5 P 0.4785(2) 0.48273(11) 0.1890(2) 0.0695(7) Uani 1 1 d . . . . .
P6 P 0.5934(2) 0.60877(12) 0.10495(17) 0.0679(7) Uani 1 1 d . . . . .
C19 C 0.9250(7) 0.4470(3) -0.3563(5) 0.065(3) Uani 0.636(7) 1 d D U P A 1
F1 F 0.9577(13) 0.3980(4) -0.3981(6) 0.097(4) Uani 0.636(7) 1 d D U P A 1
F2 F 1.0214(9) 0.4851(3) -0.3660(6) 0.101(3) Uani 0.636(7) 1 d D U P A 1
F3 F 0.8096(8) 0.4659(7) -0.4094(7) 0.160(6) Uani 0.636(7) 1 d D U P A 1
O1 O 1.0345(7) 0.4082(5) -0.1803(7) 0.095(4) Uani 0.636(7) 1 d D U P A 1
O2 O 0.7900(6) 0.3992(3) -0.2275(6) 0.059(2) Uani 0.636(7) 1 d D U P A 1
O3 O 0.8898(12) 0.4931(3) -0.1853(9) 0.102(6) Uani 0.636(7) 1 d D U P A 1
S1 S 0.9083(4) 0.43551(17) -0.2218(3) 0.0520(11) Uani 0.636(7) 1 d D U P A 1
C19A C 0.8876(11) 0.4440(5) -0.3473(7) 0.073(5) Uani 0.364(7) 1 d D U P A 2
F1A F 0.9684(17) 0.4192(9) -0.4052(8) 0.122(8) Uani 0.364(7) 1 d D U P A 2
F2A F 0.7718(12) 0.4145(6) -0.3594(11) 0.120(7) Uani 0.364(7) 1 d D U P A 2
F3A F 0.859(2) 0.4967(5) -0.3831(10) 0.106(7) Uani 0.364(7) 1 d D U P A 2
O1A O 0.9764(15) 0.3863(3) -0.1839(10) 0.078(6) Uani 0.364(7) 1 d D U P A 2
O2A O 1.0969(8) 0.4732(5) -0.2167(9) 0.069(5) Uani 0.364(7) 1 d D U P A 2
O3A O 0.8742(11) 0.4799(6) -0.1649(10) 0.047(4) Uani 0.364(7) 1 d D U P A 2
S1A S 0.9680(6) 0.4460(3) -0.2130(5) 0.0500(18) Uani 0.364(7) 1 d D U P A 2
C20 C 0.4827(6) 0.2500 0.2559(5) 0.065(3) Uani 0.791(11) 2 d DS TU P B 1
F4 F 0.5304(8) 0.2956(4) 0.3130(6) 0.137(4) Uani 0.791(11) 1 d D U P B 1
F5 F 0.3490(5) 0.2500 0.2565(5) 0.051(2) Uani 0.791(11) 2 d DS TU P B 1
O4 O 0.6792(5) 0.2500 0.1501(6) 0.052(2) Uani 0.791(11) 2 d DS TU P B 1
O5 O 0.4776(10) 0.3049(4) 0.0897(8) 0.160(5) Uani 0.791(11) 1 d D U P B 1
S2 S 0.5319(3) 0.2500 0.1333(2) 0.0793(11) Uani 0.791(11) 2 d DS TU P B 1
C20A C 0.4827(6) 0.2500 0.2559(5) 0.065(3) Uani 0.209(11) 2 d DS TU P B 2
F4A F 0.3701(14) 0.2743(12) 0.2682(9) 0.090(8) Uani 0.209(11) 1 d D U P B 2
F5A F 0.5748(12) 0.2500 0.3350(5) 0.034(6) Uani 0.209(11) 2 d DS TU P B 2
O4A O 0.4120(11) 0.2500 0.0589(7) 0.041(7) Uani 0.209(11) 2 d DS TU P B 2
O5A O 0.623(2) 0.2978(9) 0.1305(8) 0.175(13) Uani 0.209(11) 1 d D U P B 2
S2A S 0.5319(3) 0.2500 0.1333(2) 0.0793(11) Uani 0.209(11) 2 d DS TU P B 2
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'
F F 0.0171 0.0103 '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'
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
C2 C1 C6 110.7(5) . .
C2 C1 P1 109.1(5) . .
C6 C1 P1 114.4(5) . .
C3 C2 C1 111.4(6) . .
C2 C3 C4 110.4(6) . .
C5 C4 C3 111.3(6) . .
C4 C5 C6 112.2(6) . .
C5 C6 C1 111.6(6) . .
C5 C6 P2 107.3(5) . .
C1 C6 P2 111.3(4) . .
C8 C7 C12 114.1(10) . .
C8 C7 P4 112.7(7) . .
C12 C7 P4 113.0(8) . .
C7 C8 C9 117.1(10) . .
C7 C8 P3 122.3(7) . .
C9 C8 P3 117.8(8) . .
C8 C9 C10 117.1(11) . .
C11 C10 C9 117.9(15) . .
C10 C11 C12 113.7(14) . .
C11 C12 C7 120.5(12) . .
C14 C13 C18 111.4(9) . .
C14 C13 P5 112.6(6) . .
C18 C13 P5 109.8(7) . .
C15 C14 C13 109.7(7) . .
C15 C14 P6 113.0(6) . .
C13 C14 P6 112.5(7) . .
C14 C15 C16 114.8(8) . .
C17 C16 C15 109.1(11) . .
C16 C17 C18 111.9(9) . .
C13 C18 C17 111.0(8) . .
P2 Ag1 P2 122.39(10) . 4_565
P2 Ag1 P3 109.94(6) . .
P2 Ag1 P3 109.94(6) 4_565 .
P2 Ag1 P4 112.90(5) . .
P2 Ag1 P4 112.90(5) 4_565 .
P3 Ag1 P4 81.08(10) . .
P6 Ag2 P1 117.73(8) 3_665 .
P6 Ag2 P5 125.11(9) 3_665 .
P1 Ag2 P5 115.51(8) . .
P6 Ag2 Ag2 90.66(7) 3_665 3_665
P1 Ag2 Ag2 119.36(6) . 3_665
P5 Ag2 Ag2 74.41(6) . 3_665
C1 P1 Ag2 115.5(2) . .
C6 P2 Ag1 120.4(2) . .
C8 P3 Ag1 107.6(3) . .
C7 P4 C7 27.2(8) 4_565 .
C7 P4 Ag1 108.0(3) 4_565 .
C7 P4 Ag1 108.0(3) . .
C13 P5 Ag2 121.9(3) . .
C14 P6 Ag2 121.7(3) . 3_665
F3 C19 F2 107.9(5) . .
F3 C19 F1 108.1(6) . .
F2 C19 F1 107.6(5) . .
F3 C19 S1 111.2(5) . .
F2 C19 S1 111.6(5) . .
F1 C19 S1 110.3(4) . .
O1 S1 O2 114.9(4) . .
O1 S1 O3 115.5(5) . .
O2 S1 O3 114.4(4) . .
O1 S1 C19 103.2(4) . .
O2 S1 C19 103.4(3) . .
O3 S1 C19 103.1(4) . .
F1A C19A F3A 108.0(6) . .
F1A C19A F2A 107.4(6) . .
F3A C19A F2A 107.3(6) . .
F1A C19A S1A 111.1(5) . .
F3A C19A S1A 111.2(5) . .
F2A C19A S1A 111.6(5) . .
O2A S1A O1A 114.8(5) . .
O2A S1A O3A 114.6(5) . .
O1A S1A O3A 115.0(5) . .
O2A S1A C19A 103.5(4) . .
O1A S1A C19A 103.5(5) . .
O3A S1A C19A 103.2(5) . .
F5 C20 F4 105.2(4) . 4_565
F5 C20 F4 105.2(4) . .
F4 C20 F4 103.9(12) 4_565 .
F5 C20 S2 115.2(5) . .
F4 C20 S2 113.2(4) 4_565 .
F4 C20 S2 113.2(4) . .
O4 S2 O5 111.2(4) . 4_565
O4 S2 O5 111.2(4) . .
O5 S2 O5 120.6(11) 4_565 .
O4 S2 C20 106.2(4) . .
O5 S2 C20 102.9(4) 4_565 .
O5 S2 C20 102.9(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.531(9) .
C1 C6 1.540(9) .
C1 P1 1.844(6) .
C2 C3 1.523(10) .
C3 C4 1.523(12) .
C4 C5 1.518(11) .
C5 C6 1.536(10) .
C6 P2 1.853(7) .
C7 C8 1.532(5) .
C7 C12 1.537(5) .
C7 P4 1.818(13) .
C8 C9 1.536(5) .
C8 P3 1.754(13) .
C9 C10 1.537(5) .
C10 C11 1.534(5) .
C11 C12 1.537(5) .
C13 C14 1.516(14) .
C13 C18 1.530(12) .
C13 P5 1.903(10) .
C14 C15 1.492(14) .
C14 P6 1.852(9) .
C15 C16 1.524(14) .
C16 C17 1.495(17) .
C17 C18 1.531(16) .
Ag1 P2 2.477(2) .
Ag1 P2 2.477(2) 4_565
Ag1 P3 2.526(3) .
Ag1 P4 2.556(3) .
Ag2 P6 2.445(3) 3_665
Ag2 P1 2.4623(19) .
Ag2 P5 2.471(3) .
Ag2 Ag2 3.2068(14) 3_665
P4 C7 1.818(13) 4_565
P6 Ag2 2.445(3) 3_665
C19 F3 1.314(5) .
C19 F2 1.316(5) .
C19 F1 1.319(5) .
C19 S1 1.822(7) .
O1 S1 1.425(5) .
O2 S1 1.429(5) .
O3 S1 1.433(5) .
C19A F1A 1.317(6) .
C19A F3A 1.317(6) .
C19A F2A 1.319(6) .
C19A S1A 1.820(8) .
O1A S1A 1.427(5) .
O2A S1A 1.427(5) .
O3A S1A 1.434(5) .
C20 F5 1.321(5) .
C20 F4 1.334(5) 4_565
C20 F4 1.334(5) .
C20 S2 1.756(6) .
O4 S2 1.437(5) .
O5 S2 1.455(5) .
S2 O5 1.455(5) 4_565
F4A F4A 1.12(5) 4_565
