#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:43:39 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179860 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/56/7015667.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_7015667
loop_
_publ_author_name
'Siemeling, Ulrich'
'Klemann, Thorsten'
'Bruhn, Clemens'
'Schulz, Jiří'
'Štěpnička, Petr'
_publ_section_title
;
 The coordination behaviour of ferrocene-based pyridylphosphine ligands
 towards Zn(II), Cd(II) and Hg(II).
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4722
_journal_page_last               4740
_journal_paper_doi               10.1039/c0dt01810d
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C27 H22 Br2 Fe Hg N P'
_chemical_formula_sum            'C27 H22 Br2 Fe Hg N P'
_chemical_formula_weight         807.69
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                104.921(8)
_cell_angle_beta                 92.316(8)
_cell_angle_gamma                110.214(8)
_cell_formula_units_Z            2
_cell_length_a                   10.1471(10)
_cell_length_b                   10.3258(10)
_cell_length_c                   13.6179(13)
_cell_measurement_reflns_used    13800
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.66
_cell_measurement_theta_min      2.20
_cell_volume                     1280.6(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      ' 208 frames, detector distance = 135 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9514
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.56
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           30
_diffrn_source_power             1.50
_diffrn_source_voltage           50
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    9.752
_exptl_absorpt_correction_T_max  0.5998
_exptl_absorpt_correction_T_min  0.2161
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-red ver. 1.31 (Stoe & Cie. 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.095
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.628
_refine_diff_density_min         -1.305
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4485
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0224
_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)+(0.0366P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0536
_reflns_number_gt                4156
_reflns_number_total             4485
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt01810d.txt
_cod_data_source_block           i0507a
_cod_database_code               7015667
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
C1 C -0.2609(4) 0.1202(4) 0.3776(3) 0.0199(7) Uani 1 1 d . . .
C2 C -0.2932(5) -0.0227(4) 0.3898(3) 0.0244(8) Uani 1 1 d . . .
H2A H -0.3853 -0.0911 0.3874 0.029 Uiso 1 1 calc R . .
C3 C -0.1626(5) -0.0422(4) 0.4059(3) 0.0265(8) Uani 1 1 d . . .
H3A H -0.1525 -0.1263 0.4158 0.032 Uiso 1 1 calc R . .
C4 C -0.0493(5) 0.0863(4) 0.4046(3) 0.0278(9) Uani 1 1 d . . .
H4A H 0.0489 0.1020 0.4141 0.033 Uiso 1 1 calc R . .
C5 C -0.1072(4) 0.1870(4) 0.3870(3) 0.0226(8) Uani 1 1 d . . .
H5A H -0.0551 0.2807 0.3821 0.027 Uiso 1 1 calc R . .
C6 C -0.1175(4) 0.0455(4) 0.1364(3) 0.0204(7) Uani 1 1 d . . .
C7 C -0.2702(4) -0.0132(4) 0.1237(3) 0.0221(8) Uani 1 1 d . . .
H7A H -0.3317 0.0327 0.1085 0.026 Uiso 1 1 calc R . .
C8 C -0.3124(5) -0.1542(4) 0.1384(3) 0.0295(9) Uani 1 1 d . . .
H8A H -0.4074 -0.2183 0.1336 0.035 Uiso 1 1 calc R . .
C9 C -0.1891(5) -0.1818(4) 0.1611(3) 0.0309(10) Uani 1 1 d . . .
H9A H -0.1871 -0.2668 0.1748 0.037 Uiso 1 1 calc R . .
C10 C -0.0685(5) -0.0597(4) 0.1599(3) 0.0269(9) Uani 1 1 d . . .
H10A H 0.0279 -0.0496 0.1725 0.032 Uiso 1 1 calc R . .
C11 C -0.0262(4) 0.1865(4) 0.1247(3) 0.0203(7) Uani 1 1 d . . .
C12 C 0.1112(4) 0.2072(4) 0.1010(3) 0.0250(8) Uani 1 1 d . . .
H12A H 0.1494 0.1346 0.0984 0.030 Uiso 1 1 calc R . .
C13 C 0.1915(4) 0.3355(4) 0.0812(3) 0.0283(9) Uani 1 1 d . . .
H13A H 0.2854 0.3517 0.0658 0.034 Uiso 1 1 calc R . .
C14 C 0.1327(4) 0.4390(4) 0.0843(3) 0.0261(8) Uani 1 1 d . . .
H14A H 0.1841 0.5262 0.0694 0.031 Uiso 1 1 calc R . .
C15 C -0.0034(4) 0.4119(4) 0.1099(3) 0.0258(8) Uani 1 1 d . . .
H15A H -0.0436 0.4829 0.1118 0.031 Uiso 1 1 calc R . .
C16 C -0.4079(4) 0.3048(4) 0.4694(3) 0.0206(8) Uani 1 1 d . . .
C17 C -0.2884(5) 0.3870(4) 0.5439(3) 0.0282(9) Uani 1 1 d . . .
H17A H -0.1972 0.3886 0.5292 0.034 Uiso 1 1 calc R . .
C18 C -0.3033(6) 0.4670(5) 0.6404(3) 0.0365(10) Uani 1 1 d . . .
H18A H -0.2226 0.5216 0.6913 0.044 Uiso 1 1 calc R . .
C19 C -0.4360(6) 0.4660(5) 0.6612(3) 0.0354(10) Uani 1 1 d . . .
H19A H -0.4463 0.5195 0.7265 0.042 Uiso 1 1 calc R . .
C20 C -0.5542(5) 0.3867(4) 0.5867(4) 0.0344(10) Uani 1 1 d . . .
H20A H -0.6449 0.3868 0.6016 0.041 Uiso 1 1 calc R . .
C21 C -0.5413(4) 0.3068(4) 0.4899(3) 0.0263(8) Uani 1 1 d . . .
H21A H -0.6221 0.2545 0.4388 0.032 Uiso 1 1 calc R . .
C22 C -0.5473(4) 0.0553(4) 0.2882(3) 0.0219(8) Uani 1 1 d . . .
C23 C -0.5963(4) 0.0241(4) 0.1838(3) 0.0238(8) Uani 1 1 d . . .
H23A H -0.5459 0.0842 0.1447 0.029 Uiso 1 1 calc R . .
C24 C -0.7189(5) -0.0953(4) 0.1374(3) 0.0310(9) Uani 1 1 d . . .
H24A H -0.7502 -0.1188 0.0662 0.037 Uiso 1 1 calc R . .
C25 C -0.7956(5) -0.1802(4) 0.1955(4) 0.0357(10) Uani 1 1 d . . .
H25A H -0.8797 -0.2610 0.1638 0.043 Uiso 1 1 calc R . .
C26 C -0.7499(5) -0.1474(4) 0.3007(4) 0.0345(10) Uani 1 1 d . . .
H26A H -0.8033 -0.2049 0.3402 0.041 Uiso 1 1 calc R . .
C27 C -0.6264(5) -0.0307(4) 0.3465(3) 0.0294(9) Uani 1 1 d . . .
H27A H -0.5948 -0.0085 0.4176 0.035 Uiso 1 1 calc R . .
N N -0.0822(3) 0.2902(3) 0.1323(2) 0.0219(7) Uani 1 1 d . . .
P P -0.38003(10) 0.20165(9) 0.34683(7) 0.01793(19) Uani 1 1 d . . .
Fe Fe -0.18571(6) 0.00062(5) 0.26828(4) 0.01930(12) Uani 1 1 d . . .
Br1 Br -0.07987(4) 0.59051(4) 0.34909(3) 0.02411(9) Uani 1 1 d . . .
Br2 Br -0.39384(4) 0.38367(4) 0.08057(3) 0.02650(10) Uani 1 1 d . . .
Hg Hg -0.273067(14) 0.347555(13) 0.234406(10) 0.01858(6) Uani 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'
N N 0.0061 0.0033 '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'
Br Br -0.2901 2.4595 '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
C2 C1 C5 107.1(3) . . ?
C2 C1 P 128.9(3) . . ?
C5 C1 P 123.8(3) . . ?
C2 C1 Fe 69.4(2) . . ?
C5 C1 Fe 69.6(2) . . ?
P C1 Fe 122.46(19) . . ?
C3 C2 C1 108.0(3) . . ?
C3 C2 Fe 70.3(2) . . ?
C1 C2 Fe 68.8(2) . . ?
C3 C2 H2A 126.0 . . ?
C1 C2 H2A 126.0 . . ?
Fe C2 H2A 126.5 . . ?
C2 C3 C4 108.3(3) . . ?
C2 C3 Fe 69.0(2) . . ?
C4 C3 Fe 69.9(2) . . ?
C2 C3 H3A 125.9 . . ?
C4 C3 H3A 125.9 . . ?
Fe C3 H3A 126.9 . . ?
C5 C4 C3 109.0(4) . . ?
C5 C4 Fe 69.2(2) . . ?
C3 C4 Fe 69.5(2) . . ?
C5 C4 H4A 125.5 . . ?
C3 C4 H4A 125.5 . . ?
Fe C4 H4A 127.5 . . ?
C4 C5 C1 107.5(3) . . ?
C4 C5 Fe 70.3(2) . . ?
C1 C5 Fe 68.5(2) . . ?
C4 C5 H5A 126.2 . . ?
C1 C5 H5A 126.2 . . ?
Fe C5 H5A 126.5 . . ?
C10 C6 C7 107.4(3) . . ?
C10 C6 C11 125.7(4) . . ?
C7 C6 C11 126.8(3) . . ?
C10 C6 Fe 68.9(2) . . ?
C7 C6 Fe 69.9(2) . . ?
C11 C6 Fe 127.8(2) . . ?
C8 C7 C6 107.4(4) . . ?
C8 C7 Fe 69.8(2) . . ?
C6 C7 Fe 69.2(2) . . ?
C8 C7 H7A 126.3 . . ?
C6 C7 H7A 126.3 . . ?
Fe C7 H7A 126.3 . . ?
C9 C8 C7 108.7(4) . . ?
C9 C8 Fe 69.3(2) . . ?
C7 C8 Fe 69.5(2) . . ?
C9 C8 H8A 125.7 . . ?
C7 C8 H8A 125.7 . . ?
Fe C8 H8A 127.1 . . ?
C8 C9 C10 108.1(3) . . ?
C8 C9 Fe 70.5(2) . . ?
C10 C9 Fe 69.1(2) . . ?
C8 C9 H9A 125.9 . . ?
C10 C9 H9A 125.9 . . ?
Fe C9 H9A 126.0 . . ?
C9 C10 C6 108.3(4) . . ?
C9 C10 Fe 70.1(2) . . ?
C6 C10 Fe 70.0(2) . . ?
C9 C10 H10A 125.8 . . ?
C6 C10 H10A 125.8 . . ?
Fe C10 H10A 125.7 . . ?
N C11 C12 121.7(3) . . ?
N C11 C6 118.3(3) . . ?
C12 C11 C6 120.0(3) . . ?
C13 C12 C11 119.5(4) . . ?
C13 C12 H12A 120.3 . . ?
C11 C12 H12A 120.3 . . ?
C14 C13 C12 119.1(4) . . ?
C14 C13 H13A 120.4 . . ?
C12 C13 H13A 120.4 . . ?
C13 C14 C15 118.2(4) . . ?
C13 C14 H14A 120.9 . . ?
C15 C14 H14A 120.9 . . ?
N C15 C14 123.9(4) . . ?
N C15 H15A 118.1 . . ?
C14 C15 H15A 118.1 . . ?
C21 C16 C17 119.8(3) . . ?
C21 C16 P 122.7(3) . . ?
C17 C16 P 117.4(3) . . ?
C16 C17 C18 120.1(4) . . ?
C16 C17 H17A 120.0 . . ?
C18 C17 H17A 120.0 . . ?
C19 C18 C17 119.8(4) . . ?
C19 C18 H18A 120.1 . . ?
C17 C18 H18A 120.1 . . ?
C18 C19 C20 120.2(4) . . ?
C18 C19 H19A 119.9 . . ?
C20 C19 H19A 119.9 . . ?
C19 C20 C21 120.8(4) . . ?
C19 C20 H20A 119.6 . . ?
C21 C20 H20A 119.6 . . ?
C16 C21 C20 119.2(4) . . ?
C16 C21 H21A 120.4 . . ?
C20 C21 H21A 120.4 . . ?
C23 C22 C27 119.6(4) . . ?
C23 C22 P 120.3(3) . . ?
C27 C22 P 120.1(3) . . ?
C24 C23 C22 119.9(4) . . ?
C24 C23 H23A 120.1 . . ?
C22 C23 H23A 120.1 . . ?
C25 C24 C23 120.0(4) . . ?
C25 C24 H24A 120.0 . . ?
C23 C24 H24A 120.0 . . ?
C24 C25 C26 120.5(4) . . ?
C24 C25 H25A 119.7 . . ?
C26 C25 H25A 119.7 . . ?
C27 C26 C25 119.6(4) . . ?
C27 C26 H26A 120.2 . . ?
C25 C26 H26A 120.2 . . ?
C26 C27 C22 120.3(4) . . ?
C26 C27 H27A 119.9 . . ?
C22 C27 H27A 119.9 . . ?
C15 N C11 117.5(3) . . ?
C15 N Hg 107.1(2) . . ?
C11 N Hg 132.2(2) . . ?
C1 P C22 106.49(17) . . ?
C1 P C16 105.95(17) . . ?
C22 P C16 107.76(18) . . ?
C1 P Hg 107.98(12) . . ?
C22 P Hg 113.92(13) . . ?
C16 P Hg 114.18(11) . . ?
C1 Fe C2 41.82(14) . . ?
C1 Fe C10 162.77(15) . . ?
C2 Fe C10 152.73(15) . . ?
C1 Fe C5 41.86(15) . . ?
C2 Fe C5 69.91(15) . . ?
C10 Fe C5 123.38(16) . . ?
C1 Fe C9 156.16(17) . . ?
C2 Fe C9 118.36(16) . . ?
C10 Fe C9 40.77(17) . . ?
C5 Fe C9 158.72(18) . . ?
C1 Fe C6 126.92(14) . . ?
C2 Fe C6 164.59(16) . . ?
C10 Fe C6 41.13(15) . . ?
C5 Fe C6 108.56(15) . . ?
C9 Fe C6 68.84(15) . . ?
C1 Fe C3 69.45(15) . . ?
C2 Fe C3 40.74(17) . . ?
C10 Fe C3 117.27(17) . . ?
C5 Fe C3 68.95(15) . . ?
C9 Fe C3 103.77(16) . . ?
C6 Fe C3 154.16(17) . . ?
C1 Fe C4 69.16(16) . . ?
C2 Fe C4 68.70(17) . . ?
C10 Fe C4 104.94(18) . . ?
C5 Fe C4 40.52(16) . . ?
C9 Fe C4 121.28(17) . . ?
C6 Fe C4 120.73(17) . . ?
C3 Fe C4 40.62(17) . . ?
C1 Fe C7 110.30(16) . . ?
C2 Fe C7 126.50(16) . . ?
C10 Fe C7 68.81(17) . . ?
C5 Fe C7 124.24(15) . . ?
C9 Fe C7 68.53(16) . . ?
C6 Fe C7 40.89(15) . . ?
C3 Fe C7 161.19(16) . . ?
C4 Fe C7 158.04(15) . . ?
C1 Fe C8 123.25(17) . . ?
C2 Fe C8 107.53(17) . . ?
C10 Fe C8 68.08(18) . . ?
C5 Fe C8 160.25(17) . . ?
C9 Fe C8 40.16(19) . . ?
C6 Fe C8 68.43(15) . . ?
C3 Fe C8 122.63(16) . . ?
C4 Fe C8 158.24(16) . . ?
C7 Fe C8 40.72(15) . . ?
P Hg Br2 128.72(3) . . ?
P Hg N 118.87(7) . . ?
Br2 Hg N 92.37(7) . . ?
P Hg Br1 108.03(2) . . ?
Br2 Hg Br1 111.667(16) . . ?
N Hg Br1 90.12(7) . . ?
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
C1 C2 1.452(5) . ?
C1 C5 1.456(5) . ?
C1 P 1.785(4) . ?
C1 Fe 2.030(4) . ?
C2 C3 1.425(6) . ?
C2 Fe 2.038(4) . ?
C2 H2A 0.9500 . ?
C3 C4 1.429(6) . ?
C3 Fe 2.056(4) . ?
C3 H3A 0.9500 . ?
C4 C5 1.422(6) . ?
C4 Fe 2.061(4) . ?
C4 H4A 0.9500 . ?
C5 Fe 2.045(4) . ?
C5 H5A 0.9500 . ?
C6 C10 1.439(5) . ?
C6 C7 1.439(5) . ?
C6 C11 1.485(5) . ?
C6 Fe 2.055(4) . ?
C7 C8 1.438(5) . ?
C7 Fe 2.065(4) . ?
C7 H7A 0.9500 . ?
C8 C9 1.415(7) . ?
C8 Fe 2.069(4) . ?
C8 H8A 0.9500 . ?
C9 C10 1.426(6) . ?
C9 Fe 2.053(4) . ?
C9 H9A 0.9500 . ?
C10 Fe 2.040(4) . ?
C10 H10A 0.9500 . ?
C11 N 1.360(5) . ?
C11 C12 1.399(6) . ?
C12 C13 1.395(6) . ?
C12 H12A 0.9500 . ?
C13 C14 1.385(6) . ?
C13 H13A 0.9500 . ?
C14 C15 1.389(6) . ?
C14 H14A 0.9500 . ?
C15 N 1.354(5) . ?
C15 H15A 0.9500 . ?
C16 C21 1.399(6) . ?
C16 C17 1.403(6) . ?
C16 P 1.825(4) . ?
C17 C18 1.406(6) . ?
C17 H17A 0.9500 . ?
C18 C19 1.384(7) . ?
C18 H18A 0.9500 . ?
C19 C20 1.390(7) . ?
C19 H19A 0.9500 . ?
C20 C21 1.402(6) . ?
C20 H20A 0.9500 . ?
C21 H21A 0.9500 . ?
C22 C23 1.403(6) . ?
C22 C27 1.409(5) . ?
C22 P 1.817(4) . ?
C23 C24 1.394(6) . ?
C23 H23A 0.9500 . ?
C24 C25 1.391(6) . ?
C24 H24A 0.9500 . ?
C25 C26 1.403(7) . ?
C25 H25A 0.9500 . ?
C26 C27 1.385(6) . ?
C26 H26A 0.9500 . ?
C27 H27A 0.9500 . ?
N Hg 2.573(3) . ?
P Hg 2.4462(9) . ?
Br1 Hg 2.6291(5) . ?
Br2 Hg 2.5574(5) . ?
