#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:21:14 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179786 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/82/7008227.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_7008227
loop_
_publ_author_name
'Bowmaker, Graham A.'
'Assadollahzadeh, Behnam'
'Brodie, Andrew M.'
'Ainscough, Eric W.'
'Freeman, Graham H.'
'Jameson, Geoffrey B.'
_publ_section_title
;
 Structural and spectroscopic studies on mercury(II) tribenzylphosphine
 complexes.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1602
_journal_page_last               1612
_journal_paper_doi               10.1039/b419253b
_journal_year                    2005
_chemical_formula_sum            'C22 H21 Hg N2 O3 P S'
_chemical_formula_weight         625.03
_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                109.463(1)
_cell_angle_beta                 105.806(1)
_cell_angle_gamma                99.8370(10)
_cell_formula_units_Z            2
_cell_length_a                   10.4193(2)
_cell_length_b                   10.4422(2)
_cell_length_c                   11.55770(10)
_cell_measurement_reflns_used    4777
_cell_measurement_temperature    83(2)
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      2.00
_cell_volume                     1092.34(3)
_computing_cell_refinement       'Siemens SMART (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'Siemens SAINT (Siemens, 1995)'
_computing_molecular_graphics    'Siemens SHELXTL (Siemens, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      83(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Siemens SMART'
_diffrn_measurement_method       'Area dectector /w 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  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11269
_diffrn_reflns_theta_full        27.11
_diffrn_reflns_theta_max         27.11
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    7.240
_exptl_absorpt_correction_T_max  0.3904
_exptl_absorpt_correction_T_min  0.2363
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'blessing, Acta Cryst., (1995) A51, 33-38'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.900
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.551
_refine_diff_density_min         -2.030
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4777
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.059
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0334P)²+1.1432P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0596
_refine_ls_wR_factor_ref         0.0604
_reflns_number_gt                4586
_reflns_number_total             4777
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b419253b.txt
_cod_data_source_block           6_thiocyanate
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7008227
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
Hg1 Hg 0.263220(11) 0.544818(12) 0.584734(10) 0.01365(5) Uani 1 1 d . . .
S1 S 0.23476(8) 0.31493(9) 0.41615(8) 0.01446(15) Uani 1 1 d . . .
P1 P 0.27516(8) 0.67610(9) 0.80333(8) 0.01090(15) Uani 1 1 d . . .
N1 N 0.0433(3) 0.6530(3) 0.4358(3) 0.0162(6) Uani 1 1 d . . .
N2 N 0.4913(3) 0.6652(3) 0.5859(3) 0.0223(6) Uani 1 1 d . . .
O1 O 0.1534(3) 0.6276(3) 0.4168(2) 0.0212(5) Uani 1 1 d . . .
O2 O -0.0469(3) 0.6689(3) 0.3505(3) 0.0240(5) Uani 1 1 d . . .
O3 O 0.0265(3) 0.6571(3) 0.5403(2) 0.0266(6) Uani 1 1 d . . .
C1 C 0.3975(3) 0.3311(3) 0.4154(3) 0.0146(6) Uani 1 1 d . . .
C11 C 0.3817(3) 0.8589(3) 0.8673(3) 0.0146(6) Uani 1 1 d . . .
H11A H 0.3659 0.9126 0.9459 0.017 Uiso 1 1 calc R . .
H11B H 0.4788 0.8602 0.8933 0.017 Uiso 1 1 calc R . .
C12 C 0.3579(4) 0.9353(4) 0.7756(3) 0.0173(7) Uani 1 1 d . . .
C13 C 0.2314(4) 0.9625(4) 0.7283(3) 0.0228(7) Uani 1 1 d . . .
H13 H 0.1565 0.9302 0.7505 0.027 Uiso 1 1 calc R . .
C14 C 0.2165(5) 1.0376(4) 0.6480(4) 0.0345(10) Uani 1 1 d . . .
H14 H 0.1320 1.0553 0.6172 0.041 Uiso 1 1 calc R . .
C15 C 0.3272(6) 1.0858(4) 0.6143(4) 0.0378(11) Uani 1 1 d . . .
H15 H 0.3170 1.1357 0.5607 0.045 Uiso 1 1 calc R . .
C16 C 0.4533(5) 1.0600(4) 0.6602(4) 0.0326(9) Uani 1 1 d . . .
H16 H 0.5274 1.0918 0.6369 0.039 Uiso 1 1 calc R . .
C17 C 0.4687(4) 0.9862(4) 0.7413(3) 0.0234(8) Uani 1 1 d . . .
H17 H 0.5541 0.9705 0.7732 0.028 Uiso 1 1 calc R . .
C21 C 0.1070(3) 0.6760(4) 0.8247(3) 0.0144(6) Uani 1 1 d . . .
H21A H 0.0562 0.7155 0.7684 0.017 Uiso 1 1 calc R . .
H21B H 0.0527 0.5789 0.7973 0.017 Uiso 1 1 calc R . .
C22 C 0.1220(3) 0.7605(4) 0.9655(3) 0.0146(6) Uani 1 1 d . . .
C23 C 0.1295(4) 0.9034(4) 1.0087(3) 0.0185(7) Uani 1 1 d . . .
H23 H 0.1258 0.9485 0.9513 0.022 Uiso 1 1 calc R . .
C24 C 0.1427(4) 0.9800(4) 1.1386(4) 0.0236(8) Uani 1 1 d . . .
H24 H 0.1489 1.0761 1.1673 0.028 Uiso 1 1 calc R . .
C25 C 0.1466(4) 0.9136(5) 1.2243(4) 0.0266(8) Uani 1 1 d . . .
H25 H 0.1541 0.9645 1.3102 0.032 Uiso 1 1 calc R . .
C26 C 0.1393(4) 0.7705(5) 1.1818(4) 0.0243(8) Uani 1 1 d . . .
H26 H 0.1425 0.7256 1.2393 0.029 Uiso 1 1 calc R . .
C27 C 0.1274(3) 0.6943(4) 1.0529(3) 0.0181(7) Uani 1 1 d . . .
H27 H 0.1229 0.5986 1.0250 0.022 Uiso 1 1 calc R . .
C31 C 0.3648(3) 0.6026(4) 0.9146(3) 0.0147(6) Uani 1 1 d . . .
H31A H 0.3819 0.6642 1.0045 0.018 Uiso 1 1 calc R . .
H31B H 0.3059 0.5103 0.8960 0.018 Uiso 1 1 calc R . .
C32 C 0.5012(3) 0.5881(4) 0.8989(3) 0.0133(6) Uani 1 1 d . . .
C33 C 0.6261(4) 0.6936(4) 0.9819(3) 0.0186(7) Uani 1 1 d . . .
H33 H 0.6269 0.7708 1.0520 0.022 Uiso 1 1 calc R . .
C34 C 0.7494(4) 0.6831(4) 0.9594(4) 0.0233(8) Uani 1 1 d . . .
H34 H 0.8326 0.7531 1.0150 0.028 Uiso 1 1 calc R . .
C35 C 0.7489(4) 0.5690(4) 0.8547(4) 0.0220(7) Uani 1 1 d . . .
H35 H 0.8310 0.5641 0.8385 0.026 Uiso 1 1 calc R . .
C36 C 0.6256(4) 0.4616(4) 0.7737(3) 0.0218(7) Uani 1 1 d . . .
H36 H 0.6256 0.3835 0.7049 0.026 Uiso 1 1 calc R . .
C37 C 0.5025(4) 0.4714(4) 0.7960(3) 0.0166(6) Uani 1 1 d . . .
H37 H 0.4202 0.3995 0.7418 0.020 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'
S S 0.1246 0.1234 '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
P1 Hg1 S1 147.70(3) . . ?
P1 Hg1 O1 116.13(6) . . ?
S1 Hg1 O1 91.28(6) . . ?
P1 Hg1 N2 101.92(7) . . ?
S1 Hg1 N2 95.87(7) . . ?
O1 Hg1 N2 87.14(10) . . ?
P1 Hg1 O3 77.39(5) . . ?
S1 Hg1 O3 115.34(6) . . ?
O1 Hg1 O3 47.09(7) . . ?
N2 Hg1 O3 121.69(9) . . ?
P1 Hg1 O3 102.84(5) . 2_566 ?
S1 Hg1 O3 64.36(6) . 2_566 ?
O1 Hg1 O3 78.52(8) . 2_566 ?
N2 Hg1 O3 154.93(9) . 2_566 ?
O3 Hg1 O3 60.95(10) . 2_566 ?
C1 S1 Hg1 101.45(12) . . ?
C11 P1 C31 104.62(15) . . ?
C11 P1 C21 108.71(15) . . ?
C31 P1 C21 106.10(15) . . ?
C11 P1 Hg1 111.38(11) . . ?
C31 P1 Hg1 109.71(11) . . ?
C21 P1 Hg1 115.63(11) . . ?
O2 N1 O3 120.8(3) . . ?
O2 N1 O1 120.4(3) . . ?
O3 N1 O1 118.8(3) . . ?
O2 N1 Hg1 164.8(2) . . ?
O3 N1 Hg1 69.81(18) . . ?
O1 N1 Hg1 49.89(16) . . ?
C1 N2 Hg1 152.4(3) 2_666 . ?
N1 O1 Hg1 106.72(19) . . ?
N1 O3 Hg1 86.25(19) . . ?
N1 O3 Hg1 96.78(19) . 2_566 ?
Hg1 O3 Hg1 119.05(10) . 2_566 ?
N2 C1 S1 176.3(3) 2_666 . ?
C12 C11 P1 116.7(2) . . ?
C17 C12 C13 118.4(3) . . ?
C17 C12 C11 118.7(3) . . ?
C13 C12 C11 122.8(3) . . ?
C14 C13 C12 120.5(4) . . ?
C15 C14 C13 120.1(4) . . ?
C14 C15 C16 120.2(4) . . ?
C15 C16 C17 119.8(4) . . ?
C16 C17 C12 121.0(4) . . ?
C22 C21 P1 112.9(2) . . ?
C23 C22 C27 119.2(3) . . ?
C23 C22 C21 120.8(3) . . ?
C27 C22 C21 120.0(3) . . ?
C22 C23 C24 120.3(3) . . ?
C25 C24 C23 120.3(4) . . ?
C24 C25 C26 119.7(3) . . ?
C25 C26 C27 120.1(3) . . ?
C26 C27 C22 120.4(3) . . ?
C32 C31 P1 111.0(2) . . ?
C37 C32 C33 119.3(3) . . ?
C37 C32 C31 119.7(3) . . ?
C33 C32 C31 121.0(3) . . ?
C34 C33 C32 119.9(3) . . ?
C35 C34 C33 120.4(3) . . ?
C34 C35 C36 120.0(3) . . ?
C37 C36 C35 119.8(3) . . ?
C36 C37 C32 120.6(3) . . ?
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 P1 2.3958(8) . ?
Hg1 S1 2.4438(8) . ?
Hg1 O1 2.464(3) . ?
Hg1 N2 2.486(3) . ?
Hg1 O3 2.902(3) . ?
Hg1 O3 3.011(3) 2_566 ?
S1 C1 1.677(3) . ?
P1 C11 1.820(3) . ?
P1 C31 1.834(3) . ?
P1 C21 1.835(3) . ?
N1 O2 1.242(4) . ?
N1 O3 1.255(4) . ?
N1 O1 1.279(4) . ?
N2 C1 1.157(5) 2_666 ?
O3 Hg1 3.011(3) 2_566 ?
C1 N2 1.157(5) 2_666 ?
C11 C12 1.520(5) . ?
C12 C17 1.397(5) . ?
C12 C13 1.398(5) . ?
C13 C14 1.396(6) . ?
C14 C15 1.383(7) . ?
C15 C16 1.384(7) . ?
C16 C17 1.393(6) . ?
C21 C22 1.519(4) . ?
C22 C23 1.387(5) . ?
C22 C27 1.397(5) . ?
C23 C24 1.401(5) . ?
C24 C25 1.382(6) . ?
C25 C26 1.390(6) . ?
C26 C27 1.393(5) . ?
C31 C32 1.507(4) . ?
C32 C37 1.396(5) . ?
C32 C33 1.397(5) . ?
C33 C34 1.394(5) . ?
C34 C35 1.384(6) . ?
C35 C36 1.392(5) . ?
C36 C37 1.388(5) . ?
