#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:48:36 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179307 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/04/4320474.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_4320474
loop_
_publ_author_name
'Hai-Bin Song'
'Zheng-Zhi Zhang'
'Thomas C. W. Mak'
_publ_section_title
;
 2,6-Bis(diphenylphosphino)pyridine-Bridged Hetero-Polynuclear Complexes
 Consolidated by Fe\\rightarrowM (M = Ag, Hg) Dative Bonding
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5928
_journal_page_last               5933
_journal_paper_doi               10.1021/ic010426u
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C78 H62 Fe4 Hg4 N2 O14 P4'
_chemical_formula_weight         2400.94
_chemical_name_systematic
;
   ?
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.445(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.606(2)
_cell_length_b                   14.677(2)
_cell_length_c                   18.830(3)
_cell_measurement_temperature    293(2)
_cell_volume                     4014.4(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0742
_diffrn_reflns_av_sigmaI/netI    0.1224
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26906
_diffrn_reflns_theta_full        28.03
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    8.461
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.686
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.986
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       0.000008(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.774
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         9689
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.774
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_gt           0.0380
_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)+(0.0123P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0537
_refine_ls_wR_factor_ref         0.0627
_reflns_number_gt                5032
_reflns_number_total             9689
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010426u_4.cif
_cod_data_source_block           CPD4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4320474
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_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
Hg1 Hg 0.475605(17) 0.13845(2) 0.565953(17) 0.04014(9) Uani 1 1 d . . .
Hg2 Hg 0.335573(19) -0.02478(2) 0.453473(19) 0.04915(10) Uani 1 1 d . . .
Fe1 Fe 0.30147(6) 0.10641(6) 0.52836(5) 0.0317(2) Uani 1 1 d . . .
Fe2 Fe 0.65102(6) 0.16301(6) 0.62513(6) 0.0369(3) Uani 1 1 d . . .
P1 P 0.27809(11) 0.21308(12) 0.60217(10) 0.0299(4) Uani 1 1 d . . .
P2 P 0.63465(11) 0.27856(12) 0.69514(10) 0.0321(4) Uani 1 1 d . . .
N1 N 0.4587(3) 0.2457(3) 0.6733(3) 0.0303(13) Uani 1 1 d . . .
C1 C 0.3527(4) 0.0348(5) 0.6088(5) 0.046(2) Uani 1 1 d . . .
O1 O 0.3872(4) -0.0101(4) 0.6618(3) 0.0768(19) Uani 1 1 d . . .
C2 C 0.1876(5) 0.0672(5) 0.4931(4) 0.0440(19) Uani 1 1 d . . .
O2 O 0.1108(3) 0.0425(4) 0.4706(3) 0.0714(18) Uani 1 1 d . . .
C3 C 0.3037(4) 0.1757(5) 0.4526(4) 0.0418(19) Uani 1 1 d . . .
O3 O 0.3043(3) 0.2237(4) 0.4038(3) 0.0687(17) Uani 1 1 d . . .
C4 C 0.6378(5) 0.0781(6) 0.6863(5) 0.053(2) Uani 1 1 d . . .
O4 O 0.6302(4) 0.0242(4) 0.7295(4) 0.081(2) Uani 1 1 d . . .
C5 C 0.7698(5) 0.1704(5) 0.6569(5) 0.060(2) Uani 1 1 d . . .
O5 O 0.8512(3) 0.1747(4) 0.6804(4) 0.108(3) Uani 1 1 d . . .
C6 C 0.6233(5) 0.2207(5) 0.5370(5) 0.053(2) Uani 1 1 d . . .
O6 O 0.6110(4) 0.2601(4) 0.4808(3) 0.0792(19) Uani 1 1 d . . .
C7 C 0.1965(4) 0.1792(4) 0.6463(4) 0.0296(16) Uani 1 1 d . . .
C8 C 0.2223(5) 0.1255(4) 0.7112(4) 0.0447(19) Uani 1 1 d . . .
H8A H 0.2836 0.1083 0.7345 0.054 Uiso 1 1 calc R . .
C9 C 0.1604(5) 0.0974(5) 0.7419(5) 0.058(2) Uani 1 1 d . . .
H9A H 0.1804 0.0642 0.7871 0.070 Uiso 1 1 calc R . .
C10 C 0.0692(5) 0.1173(5) 0.7070(5) 0.060(2) Uani 1 1 d . . .
H10A H 0.0269 0.0975 0.7279 0.071 Uiso 1 1 calc R . .
C11 C 0.0406(4) 0.1667(6) 0.6410(5) 0.060(2) Uani 1 1 d . . .
H11A H -0.0216 0.1794 0.6161 0.072 Uiso 1 1 calc R . .
C12 C 0.1032(4) 0.1975(5) 0.6114(4) 0.046(2) Uani 1 1 d . . .
H12A H 0.0828 0.2316 0.5667 0.056 Uiso 1 1 calc R . .
C13 C 0.2321(4) 0.3225(4) 0.5573(4) 0.0368(17) Uani 1 1 d . . .
C14 C 0.2580(5) 0.4040(5) 0.5955(5) 0.059(2) Uani 1 1 d . . .
H14A H 0.3019 0.4056 0.6447 0.071 Uiso 1 1 calc R . .
C15 C 0.2169(6) 0.4840(6) 0.5587(6) 0.077(3) Uani 1 1 d . . .
H15A H 0.2358 0.5394 0.5835 0.092 Uiso 1 1 calc R . .
C16 C 0.1493(6) 0.4839(6) 0.4872(6) 0.084(3) Uani 1 1 d . . .
H16A H 0.1213 0.5378 0.4643 0.100 Uiso 1 1 calc R . .
C17 C 0.1249(5) 0.4034(6) 0.4512(5) 0.065(3) Uani 1 1 d . . .
H17A H 0.0789 0.4022 0.4030 0.077 Uiso 1 1 calc R . .
C18 C 0.1659(4) 0.3230(5) 0.4836(4) 0.051(2) Uani 1 1 d . . .
H18A H 0.1495 0.2688 0.4563 0.062 Uiso 1 1 calc R . .
C19 C 0.3799(4) 0.2482(4) 0.6858(4) 0.0309(16) Uani 1 1 d . . .
C20 C 0.3784(4) 0.2742(4) 0.7565(4) 0.0379(17) Uani 1 1 d . . .
H20A H 0.3231 0.2776 0.7645 0.046 Uiso 1 1 calc R . .
C21 C 0.4601(5) 0.2949(5) 0.8138(4) 0.049(2) Uani 1 1 d . . .
H21A H 0.4605 0.3104 0.8618 0.058 Uiso 1 1 calc R . .
C22 C 0.5409(4) 0.2930(4) 0.8013(4) 0.0398(18) Uani 1 1 d . . .
H22A H 0.5965 0.3065 0.8403 0.048 Uiso 1 1 calc R . .
C23 C 0.5381(4) 0.2706(4) 0.7291(4) 0.0299(16) Uani 1 1 d . . .
C24 C 0.6110(4) 0.3919(4) 0.6507(4) 0.0359(17) Uani 1 1 d . . .
C25 C 0.5424(5) 0.4501(5) 0.6538(4) 0.051(2) Uani 1 1 d . . .
H25A H 0.5048 0.4308 0.6795 0.061 Uiso 1 1 calc R . .
C26 C 0.5280(6) 0.5336(6) 0.6211(5) 0.068(3) Uani 1 1 d . . .
H26A H 0.4815 0.5707 0.6250 0.082 Uiso 1 1 calc R . .
C27 C 0.5812(7) 0.5633(6) 0.5826(6) 0.081(3) Uani 1 1 d . . .
H27A H 0.5713 0.6207 0.5602 0.097 Uiso 1 1 calc R . .
C28 C 0.6495(6) 0.5088(6) 0.5768(5) 0.071(3) Uani 1 1 d . . .
H28A H 0.6859 0.5289 0.5504 0.085 Uiso 1 1 calc R . .
C29 C 0.6638(5) 0.4231(5) 0.6107(4) 0.053(2) Uani 1 1 d . . .
H29A H 0.7099 0.3859 0.6063 0.064 Uiso 1 1 calc R . .
C30 C 0.7326(4) 0.2970(5) 0.7841(4) 0.0310(16) Uani 1 1 d . . .
C31 C 0.7747(4) 0.3798(5) 0.8060(4) 0.050(2) Uani 1 1 d . . .
H31A H 0.7520 0.4302 0.7748 0.060 Uiso 1 1 calc R . .
C32 C 0.8494(5) 0.3909(6) 0.8726(5) 0.065(3) Uani 1 1 d . . .
H32A H 0.8758 0.4483 0.8858 0.078 Uiso 1 1 calc R . .
C33 C 0.8843(6) 0.3198(7) 0.9184(5) 0.087(3) Uani 1 1 d . . .
H33A H 0.9341 0.3272 0.9640 0.104 Uiso 1 1 calc R . .
C34 C 0.8451(7) 0.2352(7) 0.8969(6) 0.132(5) Uani 1 1 d . . .
H34A H 0.8694 0.1850 0.9279 0.159 Uiso 1 1 calc R . .
C35 C 0.7713(6) 0.2242(6) 0.8310(5) 0.102(4) Uani 1 1 d . . .
H35A H 0.7464 0.1664 0.8173 0.122 Uiso 1 1 calc R . .
O7 O 0.9955(9) 0.4474(9) 0.6820(6) 0.170(4) Uani 1 1 d . . .
C36 C 0.9806(10) 0.3835(10) 0.7233(15) 0.154(7) Uani 1 1 d . . .
H36A H 0.9555 0.3300 0.6925 0.185 Uiso 1 1 calc R . .
H36B H 0.9376 0.4039 0.7463 0.185 Uiso 1 1 calc R . .
C37 C 1.0712(17) 0.3627(11) 0.7828(8) 0.169(8) Uani 1 1 d . . .
H37A H 1.0728 0.3815 0.8327 0.203 Uiso 1 1 calc R . .
H37B H 1.0842 0.2980 0.7841 0.203 Uiso 1 1 calc R . .
C38 C 1.1348(11) 0.4127(13) 0.7618(12) 0.207(10) Uani 1 1 d . . .
H38A H 1.1659 0.4569 0.8011 0.248 Uiso 1 1 calc R . .
H38B H 1.1807 0.3721 0.7557 0.248 Uiso 1 1 calc R . .
C39 C 1.0873(13) 0.4564(9) 0.6938(11) 0.151(6) Uani 1 1 d . . .
H39B H 1.1044 0.5203 0.6970 0.181 Uiso 1 1 calc R . .
H39A H 1.1009 0.4287 0.6523 0.181 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'
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hg Hg -2.3894 9.2266 '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
Fe2 Hg1 Fe1 170.80(4) . . ?
Fe2 Hg1 N1 88.48(10) . . ?
Fe1 Hg1 N1 85.93(10) . . ?
Fe2 Hg1 Hg2 134.89(2) . . ?
Fe1 Hg1 Hg2 48.08(2) . . ?
N1 Hg1 Hg2 132.18(10) . . ?
Fe1 Hg2 Fe2 172.80(3) . 3_656 ?
Fe1 Hg2 Hg1 48.92(2) . . ?
Fe2 Hg2 Hg1 138.21(2) 3_656 . ?
C2 Fe1 C3 101.5(3) . . ?
C2 Fe1 C1 102.0(3) . . ?
C3 Fe1 C1 153.6(3) . . ?
C2 Fe1 P1 95.4(2) . . ?
C3 Fe1 P1 99.0(2) . . ?
C1 Fe1 P1 90.5(2) . . ?
C2 Fe1 Hg2 86.0(2) . . ?
C3 Fe1 Hg2 85.3(2) . . ?
C1 Fe1 Hg2 84.6(2) . . ?
P1 Fe1 Hg2 175.07(7) . . ?
C2 Fe1 Hg1 169.0(2) . . ?
C3 Fe1 Hg1 77.7(2) . . ?
C1 Fe1 Hg1 76.9(2) . . ?
P1 Fe1 Hg1 95.60(5) . . ?
Hg2 Fe1 Hg1 83.00(3) . . ?
C5 Fe2 C4 100.7(4) . . ?
C5 Fe2 C6 99.1(4) . . ?
C4 Fe2 C6 154.9(3) . . ?
C5 Fe2 P2 95.1(2) . . ?
C4 Fe2 P2 94.9(3) . . ?
C6 Fe2 P2 98.6(3) . . ?
C5 Fe2 Hg2 86.9(2) . 3_656 ?
C4 Fe2 Hg2 82.6(2) . 3_656 ?
C6 Fe2 Hg2 83.1(3) . 3_656 ?
P2 Fe2 Hg2 177.11(7) . 3_656 ?
C5 Fe2 Hg1 173.2(2) . . ?
C4 Fe2 Hg1 79.8(2) . . ?
C6 Fe2 Hg1 78.7(2) . . ?
P2 Fe2 Hg1 91.66(5) . . ?
Hg2 Fe2 Hg1 86.43(3) 3_656 . ?
C7 P1 C13 103.1(3) . . ?
C7 P1 C19 102.3(3) . . ?
C13 P1 C19 102.6(3) . . ?
C7 P1 Fe1 113.3(2) . . ?
C13 P1 Fe1 117.2(2) . . ?
C19 P1 Fe1 116.3(2) . . ?
C30 P2 C24 104.1(3) . . ?
C30 P2 C23 102.0(3) . . ?
C24 P2 C23 99.3(3) . . ?
C30 P2 Fe2 114.7(2) . . ?
C24 P2 Fe2 118.0(2) . . ?
C23 P2 Fe2 116.3(2) . . ?
C19 N1 C23 119.9(6) . . ?
C19 N1 Hg1 120.4(4) . . ?
C23 N1 Hg1 115.8(4) . . ?
O1 C1 Fe1 178.6(7) . . ?
O2 C2 Fe1 178.3(7) . . ?
O3 C3 Fe1 177.8(7) . . ?
O4 C4 Fe2 177.1(8) . . ?
O5 C5 Fe2 178.3(8) . . ?
O6 C6 Fe2 175.6(7) . . ?
C8 C7 C12 116.3(6) . . ?
C8 C7 P1 122.1(5) . . ?
C12 C7 P1 121.2(5) . . ?
C9 C8 C7 121.8(7) . . ?
C8 C9 C10 120.6(8) . . ?
C9 C10 C11 119.2(7) . . ?
C10 C11 C12 120.2(7) . . ?
C11 C12 C7 121.8(7) . . ?
C14 C13 C18 118.9(6) . . ?
C14 C13 P1 121.9(6) . . ?
C18 C13 P1 119.1(5) . . ?
C13 C14 C15 118.5(7) . . ?
C16 C15 C14 122.3(8) . . ?
C17 C16 C15 118.0(8) . . ?
C16 C17 C18 122.0(8) . . ?
C17 C18 C13 120.1(7) . . ?
N1 C19 C20 121.0(6) . . ?
N1 C19 P1 113.6(5) . . ?
C20 C19 P1 125.4(5) . . ?
C21 C20 C19 118.6(6) . . ?
C22 C21 C20 120.8(7) . . ?
C21 C22 C23 118.4(6) . . ?
N1 C23 C22 121.3(6) . . ?
N1 C23 P2 112.4(5) . . ?
C22 C23 P2 126.1(5) . . ?
C29 C24 C25 116.3(7) . . ?
C29 C24 P2 119.1(6) . . ?
C25 C24 P2 124.6(6) . . ?
C26 C25 C24 122.8(8) . . ?
C25 C26 C27 120.0(9) . . ?
C26 C27 C28 120.1(8) . . ?
C27 C28 C29 119.4(8) . . ?
C24 C29 C28 121.4(8) . . ?
C31 C30 C35 116.4(6) . . ?
C31 C30 P2 123.7(5) . . ?
C35 C30 P2 119.7(5) . . ?
C30 C31 C32 122.2(7) . . ?
C33 C32 C31 120.4(8) . . ?
C32 C33 C34 118.8(8) . . ?
C35 C34 C33 120.8(9) . . ?
C34 C35 C30 121.3(8) . . ?
C36 O7 C39 112.3(12) . . ?
O7 C36 C37 105.9(13) . . ?
C38 C37 C36 104.9(14) . . ?
C39 C38 C37 108.0(14) . . ?
O7 C39 C38 106.2(14) . . ?
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
Hg1 Fe2 2.5760(9) . ?
Hg1 Fe1 2.5886(9) . ?
Hg1 N1 2.650(5) . ?
Hg1 Hg2 3.4083(5) . ?
Hg2 Fe1 2.5549(10) . ?
Hg2 Fe2 2.5645(10) 3_656 ?
Fe1 C2 1.751(7) . ?
Fe1 C3 1.763(8) . ?
Fe1 C1 1.776(8) . ?
Fe1 P1 2.211(2) . ?
Fe2 C5 1.730(7) . ?
Fe2 C4 1.759(10) . ?
Fe2 C6 1.771(9) . ?
Fe2 P2 2.219(2) . ?
Fe2 Hg2 2.5645(10) 3_656 ?
P1 C7 1.825(6) . ?
P1 C13 1.834(7) . ?
P1 C19 1.855(6) . ?
P2 C30 1.829(6) . ?
P2 C24 1.838(7) . ?
P2 C23 1.843(6) . ?
N1 C19 1.334(7) . ?
N1 C23 1.350(7) . ?
C1 O1 1.152(8) . ?
C2 O2 1.173(7) . ?
C3 O3 1.161(8) . ?
C4 O4 1.174(9) . ?
C5 O5 1.184(7) . ?
C6 O6 1.158(9) . ?
C7 C8 1.385(8) . ?
C7 C12 1.387(8) . ?
C8 C9 1.358(9) . ?
C9 C10 1.364(9) . ?
C10 C11 1.365(10) . ?
C11 C12 1.366(9) . ?
C13 C14 1.379(9) . ?
C13 C18 1.394(9) . ?
C14 C15 1.395(10) . ?
C15 C16 1.374(11) . ?
C16 C17 1.345(11) . ?
C17 C18 1.375(9) . ?
C19 C20 1.393(8) . ?
C20 C21 1.370(8) . ?
C21 C22 1.366(8) . ?
C22 C23 1.384(8) . ?
C24 C29 1.384(9) . ?
C24 C25 1.387(9) . ?
C25 C26 1.354(9) . ?
C26 C27 1.359(12) . ?
C27 C28 1.368(11) . ?
C28 C29 1.392(10) . ?
C30 C31 1.372(8) . ?
C30 C35 1.377(9) . ?
C31 C32 1.373(9) . ?
C32 C33 1.338(10) . ?
C33 C34 1.378(11) . ?
C34 C35 1.359(11) . ?
O7 C36 1.292(15) . ?
O7 C39 1.374(13) . ?
C36 C37 1.479(17) . ?
C37 C38 1.402(19) . ?
C38 C39 1.382(17) . ?
