#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/29/4312957.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_4312957
loop_
_publ_author_name
'Li-Yi Zhang'
'Lin-Xi Shi'
'Zhong-Ning Chen'
_publ_contact_author
;
Zhong-Ning Chen
Fujian Institute of Research on the Structure of Matter, 
Chinese Academy of Sciences, Fuzhou, Fujian 350002, China.
;
_publ_contact_author_email       '  czn@ms.fjirsm.ac.cn '
_publ_section_title
;
 Syntheses, Structures, and Electronic Interactions of
 Dicyanamide/Tricyanomethanide-Bridged Binuclear Organometallic Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              633
_journal_page_last               640
_journal_paper_doi               10.1021/ic025879t
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C33.5 H29 F1.5 Fe N1.5 O1.5 P2 S0.5'
_chemical_formula_weight         638.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 93.3480(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.4730(2)
_cell_length_b                   18.0376(3)
_cell_length_c                   20.86220(10)
_cell_measurement_reflns_used    4502
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.49
_cell_measurement_theta_min      1.68
_cell_volume                     6188.28(13)
_computing_cell_refinement       'Siemens SMART & SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens XPREP'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       'phi and omega 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  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9759
_diffrn_reflns_theta_full        24.49
_diffrn_reflns_theta_max         24.49
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.664
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  .7868
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'deep red'
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'polydral pyramid'
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .40
_exptl_crystal_size_min          .26
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         5121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0678
_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)+(0.0591P)²+29.5727P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1569
_refine_ls_wR_factor_ref         0.1832
_reflns_number_gt                3811
_reflns_number_total             5121
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025879t-6_s1_6.cif
_cod_data_source_block           6(Compound9CF3SO3)
_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_original_formula_sum        'C33.50 H29 F1.50 Fe N1.50 O1.50 P2 S0.50'
_cod_database_code               4312957
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Fe Fe 0.53773(4) 0.30366(4) 0.56517(3) 0.0479(2) Uani 1 1 d . . .
P1 P 0.54182(8) 0.18977(8) 0.52749(7) 0.0516(4) Uani 1 1 d . . .
P2 P 0.40501(8) 0.29773(7) 0.54709(7) 0.0483(3) Uani 1 1 d . . .
N1 N 0.5287(3) 0.2572(2) 0.6465(2) 0.0507(10) Uani 1 1 d . . .
N2 N 0.5000 0.0494(7) 0.7500 0.296(14) Uani 1 2 d S . .
C1 C 0.5167(3) 0.2285(3) 0.6941(3) 0.0523(13) Uani 1 1 d . . .
C2 C 0.5000 0.1129(7) 0.7500 0.188(10) Uani 1 2 d S . .
C3 C 0.5000 0.1906(4) 0.7500 0.070(2) Uani 1 2 d S . .
C4 C 0.4384(3) 0.1507(3) 0.5319(3) 0.0600(14) Uani 1 1 d . . .
H4A H 0.4328 0.1059 0.5062 0.072 Uiso 1 1 calc R . .
H4B H 0.4279 0.1385 0.5759 0.072 Uiso 1 1 calc R . .
C5 C 0.3791(3) 0.2098(3) 0.5059(3) 0.0598(14) Uani 1 1 d . . .
H5A H 0.3238 0.1955 0.5138 0.072 Uiso 1 1 calc R . .
H5B H 0.3832 0.2154 0.4600 0.072 Uiso 1 1 calc R . .
C11 C 0.5628(3) 0.1687(3) 0.4442(3) 0.0586(14) Uani 1 1 d . . .
C12 C 0.5791(4) 0.0968(4) 0.4256(3) 0.0791(19) Uani 1 1 d . . .
H12A H 0.5847 0.0597 0.4565 0.095 Uiso 1 1 calc R . .
C13 C 0.5874(5) 0.0795(5) 0.3621(4) 0.094(2) Uani 1 1 d . . .
H13A H 0.5979 0.0307 0.3507 0.112 Uiso 1 1 calc R . .
C14 C 0.5804(5) 0.1323(5) 0.3162(4) 0.098(2) Uani 1 1 d . . .
H14A H 0.5854 0.1199 0.2733 0.117 Uiso 1 1 calc R . .
C15 C 0.5658(6) 0.2039(5) 0.3331(4) 0.114(3) Uani 1 1 d . . .
H15A H 0.5620 0.2406 0.3017 0.136 Uiso 1 1 calc R . .
C16 C 0.5568(5) 0.2226(4) 0.3974(3) 0.086(2) Uani 1 1 d . . .
H16A H 0.5466 0.2715 0.4085 0.103 Uiso 1 1 calc R . .
C21 C 0.6079(4) 0.1257(3) 0.5737(3) 0.0615(15) Uani 1 1 d . . .
C22 C 0.6865(4) 0.1479(4) 0.5901(4) 0.089(2) Uani 1 1 d . . .
H22A H 0.7045 0.1938 0.5764 0.106 Uiso 1 1 calc R . .
C23 C 0.7392(5) 0.1031(6) 0.6268(4) 0.117(3) Uani 1 1 d . . .
H23A H 0.7923 0.1184 0.6367 0.140 Uiso 1 1 calc R . .
C24 C 0.7125(7) 0.0354(6) 0.6486(4) 0.121(4) Uani 1 1 d . . .
H24A H 0.7472 0.0053 0.6740 0.145 Uiso 1 1 calc R . .
C25 C 0.6351(7) 0.0133(5) 0.6326(4) 0.119(3) Uani 1 1 d . . .
H25A H 0.6171 -0.0323 0.6469 0.142 Uiso 1 1 calc R . .
C26 C 0.5830(5) 0.0577(4) 0.5953(4) 0.090(2) Uani 1 1 d . . .
H26A H 0.5304 0.0414 0.5847 0.108 Uiso 1 1 calc R . .
C31 C 0.3487(3) 0.2970(3) 0.6197(3) 0.0574(14) Uani 1 1 d . . .
C32 C 0.3654(4) 0.3518(4) 0.6649(3) 0.0682(16) Uani 1 1 d . . .
H32A H 0.4048 0.3874 0.6578 0.082 Uiso 1 1 calc R . .
C33 C 0.3234(4) 0.3541(5) 0.7208(3) 0.085(2) Uani 1 1 d . . .
H33A H 0.3334 0.3919 0.7505 0.102 Uiso 1 1 calc R . .
C34 C 0.2672(5) 0.3000(6) 0.7318(4) 0.111(3) Uani 1 1 d . . .
H34A H 0.2388 0.3014 0.7690 0.133 Uiso 1 1 calc R . .
C35 C 0.2529(6) 0.2446(6) 0.6889(4) 0.125(3) Uani 1 1 d . . .
H35A H 0.2162 0.2073 0.6976 0.149 Uiso 1 1 calc R . .
C36 C 0.2924(4) 0.2428(5) 0.6320(3) 0.091(2) Uani 1 1 d . . .
H36A H 0.2810 0.2053 0.6022 0.109 Uiso 1 1 calc R . .
C41 C 0.3520(3) 0.3670(3) 0.4968(3) 0.0515(13) Uani 1 1 d . . .
C42 C 0.2956(3) 0.4161(3) 0.5198(3) 0.0626(15) Uani 1 1 d . . .
H42A H 0.2840 0.4144 0.5629 0.075 Uiso 1 1 calc R . .
C43 C 0.2569(4) 0.4670(4) 0.4800(3) 0.0744(17) Uani 1 1 d . . .
H43A H 0.2192 0.4991 0.4965 0.089 Uiso 1 1 calc R . .
C44 C 0.2725(4) 0.4713(3) 0.4169(4) 0.0737(18) Uani 1 1 d . . .
H44A H 0.2454 0.5058 0.3903 0.088 Uiso 1 1 calc R . .
C45 C 0.3290(4) 0.4241(4) 0.3927(3) 0.0722(17) Uani 1 1 d . . .
H45A H 0.3404 0.4268 0.3496 0.087 Uiso 1 1 calc R . .
C46 C 0.3686(4) 0.3728(3) 0.4324(3) 0.0639(15) Uani 1 1 d . . .
H46A H 0.4070 0.3415 0.4158 0.077 Uiso 1 1 calc R . .
C51 C 0.5690(4) 0.3841(3) 0.4995(3) 0.0697(17) Uani 1 1 d . . .
H51A H 0.5469 0.3893 0.4551 0.084 Uiso 1 1 calc R . .
C52 C 0.5396(4) 0.4185(3) 0.5541(3) 0.0661(16) Uani 1 1 d . . .
H52A H 0.4922 0.4513 0.5544 0.079 Uiso 1 1 calc R . .
C53 C 0.5893(4) 0.3985(4) 0.6075(3) 0.0750(18) Uani 1 1 d . . .
H53A H 0.5833 0.4150 0.6518 0.090 Uiso 1 1 calc R . .
C54 C 0.6509(4) 0.3514(4) 0.5865(4) 0.079(2) Uani 1 1 d . . .
H54A H 0.6954 0.3297 0.6135 0.094 Uiso 1 1 calc R . .
C55 C 0.6382(4) 0.3429(4) 0.5206(4) 0.0779(19) Uani 1 1 d . . .
H55A H 0.6724 0.3138 0.4931 0.093 Uiso 1 1 calc R . .
S S 0.9616(3) 0.0705(4) 0.7265(2) 0.1504(19) Uani 0.50 1 d P . .
C C 0.9616(3) 0.0705(4) 0.7265(2) 0.1504(19) Uani 0.50 1 d P . .
O1 O 0.9211(7) 0.1352(6) 0.7553(6) 0.299(8) Uani 0.50 1 d P . .
O2 O 0.9689(4) 0.0731(6) 0.6680(3) 0.216(4) Uani 0.50 1 d P . .
O3 O 0.9116(7) 0.0147(5) 0.7482(4) 0.243(5) Uani 0.50 1 d P . .
F1 F 0.9211(7) 0.1352(6) 0.7553(6) 0.299(8) Uani 0.50 1 d P . .
F2 F 0.9689(4) 0.0731(6) 0.6680(3) 0.216(4) Uani 0.50 1 d P . .
F3 F 0.9116(7) 0.0147(5) 0.7482(4) 0.243(5) Uani 0.50 1 d P . .
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'
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'
S S 0.1246 0.1234 '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'
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
N1 Fe C55 131.0(2) . . ?
N1 Fe C54 96.1(2) . . ?
C55 Fe C54 39.1(3) . . ?
N1 Fe C51 158.1(2) . . ?
C55 Fe C51 39.7(2) . . ?
C54 Fe C51 66.3(3) . . ?
N1 Fe C53 92.0(2) . . ?
C55 Fe C53 66.0(3) . . ?
C54 Fe C53 39.7(3) . . ?
C51 Fe C53 66.2(3) . . ?
N1 Fe C52 122.5(2) . . ?
C55 Fe C52 66.0(3) . . ?
C54 Fe C52 66.0(3) . . ?
C51 Fe C52 39.5(2) . . ?
C53 Fe C52 39.0(2) . . ?
N1 Fe P2 90.16(13) . . ?
C55 Fe P2 138.8(2) . . ?
C54 Fe P2 158.0(2) . . ?
C51 Fe P2 101.71(19) . . ?
C53 Fe P2 119.3(2) . . ?
C52 Fe P2 92.87(17) . . ?
N1 Fe P1 85.05(13) . . ?
C55 Fe P1 96.7(2) . . ?
C54 Fe P1 114.7(2) . . ?
C51 Fe P1 113.7(2) . . ?
C53 Fe P1 153.8(2) . . ?
C52 Fe P1 152.44(19) . . ?
P2 Fe P1 86.81(6) . . ?
C21 P1 C11 103.3(3) . . ?
C21 P1 C4 104.8(3) . . ?
C11 P1 C4 101.1(3) . . ?
C21 P1 Fe 115.6(2) . . ?
C11 P1 Fe 122.9(2) . . ?
C4 P1 Fe 106.89(18) . . ?
C31 P2 C41 103.5(3) . . ?
C31 P2 C5 105.4(3) . . ?
C41 P2 C5 103.4(3) . . ?
C31 P2 Fe 114.00(19) . . ?
C41 P2 Fe 120.22(17) . . ?
C5 P2 Fe 108.83(18) . . ?
C1 N1 Fe 174.4(4) . . ?
N1 C1 C3 177.0(6) . . ?
N2 C2 C3 180.000(3) . . ?
C1 C3 C1 121.3(7) 2_656 . ?
C1 C3 C2 119.4(4) 2_656 . ?
C1 C3 C2 119.4(4) . . ?
C5 C4 P1 106.8(4) . . ?
C4 C5 P2 108.1(4) . . ?
C16 C11 C12 118.0(6) . . ?
C16 C11 P1 121.1(5) . . ?
C12 C11 P1 120.7(5) . . ?
C13 C12 C11 121.0(7) . . ?
C14 C13 C12 120.9(7) . . ?
C13 C14 C15 119.6(7) . . ?
C14 C15 C16 120.4(7) . . ?
C11 C16 C15 120.2(7) . . ?
C26 C21 C22 118.0(6) . . ?
C26 C21 P1 123.9(5) . . ?
C22 C21 P1 118.1(5) . . ?
C21 C22 C23 121.1(8) . . ?
C22 C23 C24 119.9(9) . . ?
C25 C24 C23 119.2(8) . . ?
C24 C25 C26 120.9(9) . . ?
C21 C26 C25 121.0(8) . . ?
C32 C31 C36 119.2(6) . . ?
C32 C31 P2 118.2(4) . . ?
C36 C31 P2 122.6(5) . . ?
C31 C32 C33 120.3(6) . . ?
C34 C33 C32 119.4(7) . . ?
C35 C34 C33 120.5(7) . . ?
C34 C35 C36 120.7(8) . . ?
C31 C36 C35 119.7(7) . . ?
C46 C41 C42 117.3(5) . . ?
C46 C41 P2 119.6(4) . . ?
C42 C41 P2 123.0(4) . . ?
C43 C42 C41 121.0(6) . . ?
C44 C43 C42 121.2(6) . . ?
C43 C44 C45 119.3(6) . . ?
C44 C45 C46 120.0(6) . . ?
C45 C46 C41 121.2(6) . . ?
C52 C51 C55 106.8(6) . . ?
C52 C51 Fe 70.4(3) . . ?
C55 C51 Fe 69.7(3) . . ?
C53 C52 C51 108.6(6) . . ?
C53 C52 Fe 70.5(3) . . ?
C51 C52 Fe 70.1(3) . . ?
C52 C53 C54 107.9(6) . . ?
C52 C53 Fe 70.5(3) . . ?
C54 C53 Fe 69.9(4) . . ?
C55 C54 C53 107.7(6) . . ?
C55 C54 Fe 70.2(3) . . ?
C53 C54 Fe 70.4(3) . . ?
C54 C55 C51 108.9(6) . . ?
C54 C55 Fe 70.7(4) . . ?
C51 C55 Fe 70.6(3) . . ?
O2 S O3 116.3(8) . . ?
O2 S O1 116.2(8) . . ?
O3 S O1 98.6(6) . . ?
O2 S C 120.0(6) . 2_756 ?
O3 S C 105.7(6) . 2_756 ?
O1 S C 96.5(7) . 2_756 ?
O2 S S 120.0(6) . 2_756 ?
O3 S S 105.7(6) . 2_756 ?
O1 S S 96.5(7) . 2_756 ?
C S S 0.0(3) 2_756 2_756 ?
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
Fe N1 1.906(4) . ?
Fe C55 2.070(6) . ?
Fe C54 2.078(6) . ?
Fe C51 2.081(5) . ?
Fe C53 2.084(6) . ?
Fe C52 2.084(6) . ?
Fe P2 2.1994(15) . ?
Fe P1 2.2019(16) . ?
P1 C21 1.823(6) . ?
P1 C11 1.831(6) . ?
P1 C4 1.852(5) . ?
P2 C31 1.821(5) . ?
P2 C41 1.822(5) . ?
P2 C5 1.842(5) . ?
N1 C1 1.148(6) . ?
N2 C2 1.145(15) . ?
C1 C3 1.392(7) . ?
C2 C3 1.403(14) . ?
C3 C1 1.392(7) 2_656 ?
C4 C5 1.524(7) . ?
C11 C16 1.377(8) . ?
C11 C12 1.385(8) . ?
C12 C13 1.375(9) . ?
C13 C14 1.352(10) . ?
C14 C15 1.364(11) . ?
C15 C16 1.399(9) . ?
C21 C26 1.379(9) . ?
C21 C22 1.380(9) . ?
C22 C23 1.383(10) . ?
C23 C24 1.384(13) . ?
C24 C25 1.358(13) . ?
C25 C26 1.380(10) . ?
C31 C32 1.382(8) . ?
C31 C36 1.383(8) . ?
C32 C33 1.391(9) . ?
C33 C34 1.374(11) . ?
C34 C35 1.353(12) . ?
C35 C36 1.387(10) . ?
C41 C46 1.389(8) . ?
C41 C42 1.390(7) . ?
C42 C43 1.370(8) . ?
C43 C44 1.358(9) . ?
C44 C45 1.379(9) . ?
C45 C46 1.380(8) . ?
C51 C52 1.408(9) . ?
C51 C55 1.409(9) . ?
C52 C53 1.392(8) . ?
C53 C54 1.412(9) . ?
C54 C55 1.388(9) . ?
S O2 1.234(7) . ?
S O3 1.393(8) . ?
S O1 1.488(10) . ?
S C 1.555(10) 2_756 ?
S S 1.555(10) 2_756 ?
