#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:30:08 +0100 (vie 25 de mar de 2016) $
#$Revision: 179793 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/89/7008966.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_7008966
loop_
_publ_author_name
'Priimov, Gleb U.'
'Moore, Peter'
'Maritim, Philip K.'
'Butalanyi, Pamela K.'
'Alcock, Nathaniel W.'
_publ_section_title
;
 Synthesis of two covalently linked bis(2,2':6',2″-terpyridine)
 (terpy) chelating ligands with different length spacers, comparison of
 the crystal structures of their mononuclear nickel(II) complexes, and
 kinetic and mechanistic studies of the reaction of one ligand with
 [Fe(terpy)2]2+
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              445
_journal_paper_doi               10.1039/a907543g
_journal_year                    2000
_chemical_formula_sum            'C39 H36 F12 N8 Ni P2 S2'
_chemical_formula_weight         1028.52
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 99.644(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4137(10)
_cell_length_b                   26.0069(10)
_cell_length_c                   13.3715(10)
_cell_measurement_reflns_used    7977
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     4255.9(5)
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_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  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12791
_diffrn_reflns_theta_max         28.52
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.724
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'deep red'
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2092
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.986
_refine_ls_goodness_of_fit_obs   1.056
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4992
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_restrained_S_obs      1.056
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_obs          0.0397
_refine_ls_shift/esd_max         0.029
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0690P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1134
_refine_ls_wR_factor_obs         0.1036
_reflns_number_observed          3700
_reflns_number_total             4992
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a907543g.txt
_cod_data_source_block           pkm5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_geom_angle_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (9
times).

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (5 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7008966
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ni1 Ni 0.5000 0.344834(14) 0.2500 0.02623(12) Uani 1 d S .
S1 S 0.44519(5) 0.55945(2) 0.39893(5) 0.04302(17) Uani 1 d . .
N1 N 0.58582(15) 0.28937(6) 0.17877(13) 0.0301(4) Uani 1 d . .
C2 C 0.68185(19) 0.26717(9) 0.21508(17) 0.0372(5) Uani 1 d . .
H2A H 0.7186 0.2773 0.2802 0.045 Uiso 1 calc R .
C3 C 0.7298(2) 0.23056(9) 0.16309(19) 0.0435(6) Uani 1 d . .
H3A H 0.7981 0.2158 0.1916 0.052 Uiso 1 calc R .
C4 C 0.6771(2) 0.21576(10) 0.0689(2) 0.0479(6) Uani 1 d . .
H4A H 0.7081 0.1902 0.0316 0.057 Uiso 1 calc R .
C5 C 0.5785(2) 0.23833(9) 0.02906(19) 0.0427(6) Uani 1 d . .
H5A H 0.5410 0.2287 -0.0361 0.051 Uiso 1 calc R .
C6 C 0.53522(18) 0.27524(8) 0.08552(16) 0.0303(5) Uani 1 d . .
C7 C 0.43113(18) 0.30249(8) 0.04915(15) 0.0305(4) Uani 1 d . .
N8 N 0.40746(14) 0.33919(6) 0.11253(12) 0.0274(4) Uani 1 d . .
C9 C 0.31490(17) 0.36683(8) 0.09208(15) 0.0293(4) Uani 1 d . .
C10 C 0.24000(19) 0.35789(8) 0.00497(16) 0.0353(5) Uani 1 d . .
H10A H 0.1739 0.3769 -0.0089 0.042 Uiso 1 calc R .
C11 C 0.2639(2) 0.32049(9) -0.06143(17) 0.0406(5) Uani 1 d . .
H11A H 0.2138 0.3139 -0.1219 0.049 Uiso 1 calc R .
C12 C 0.3598(2) 0.29260(9) -0.04083(17) 0.0385(5) Uani 1 d . .
H12A H 0.3767 0.2673 -0.0870 0.046 Uiso 1 calc R .
C13 C 0.30493(18) 0.40601(8) 0.17139(16) 0.0302(4) Uani 1 d . .
N14 N 0.38246(14) 0.40256(6) 0.25526(12) 0.0302(4) Uani 1 d . .
C15 C 0.38421(19) 0.43854(8) 0.32769(17) 0.0340(5) Uani 1 d . .
H15A H 0.4379 0.4359 0.3871 0.041 Uiso 1 calc R .
C16 C 0.31091(19) 0.47955(9) 0.31965(17) 0.0361(5) Uani 1 d . .
C17 C 0.2310(2) 0.48156(9) 0.23457(18) 0.0410(6) Uani 1 d . .
H17A H 0.1783 0.5084 0.2273 0.049 Uiso 1 calc R .
C18 C 0.22751(19) 0.44446(9) 0.15971(19) 0.0399(5) Uani 1 d . .
H18A H 0.1725 0.4455 0.1011 0.048 Uiso 1 calc R .
C19 C 0.3244(2) 0.52029(9) 0.40086(19) 0.0421(6) Uani 1 d . .
H19A H 0.3297 0.5036 0.4681 0.051 Uiso 1 calc R .
H19B H 0.2590 0.5427 0.3910 0.051 Uiso 1 calc R .
C20 C 0.4052(2) 0.59124(10) 0.27709(19) 0.0443(6) Uani 1 d . .
H20A H 0.3831 0.5651 0.2238 0.053 Uiso 1 calc R .
H20B H 0.3418 0.6139 0.2800 0.053 Uiso 1 calc R .
C21 C 0.5000 0.62324(14) 0.2500 0.0495(9) Uani 1 d S .
H21A H 0.4716 0.6457 0.1918 0.059 Uiso 0.5 calc PR .
H21B H 0.5284 0.6457 0.3082 0.059 Uiso 0.5 calc PR .
P1 P 0.5000 0.10572(4) 0.2500 0.0454(2) Uani 1 d S .
F11 F 0.62559(13) 0.10512(7) 0.23911(15) 0.0731(5) Uani 1 d . .
F12A F 0.4757(2) 0.06075(14) 0.1689(2) 0.1212(17) Uani 0.904(7) d P .
F13A F 0.47624(17) 0.14672(12) 0.1647(2) 0.1153(17) Uani 0.904(7) d P .
F12B F 0.4804(17) 0.0953(10) 0.1464(15) 0.062(7) Uiso 0.096(7) d P .
F13B F 0.5000 0.1673(9) 0.2500 0.054(8) Uiso 0.096(7) d SP .
F14B F 0.5000 0.0521(10) 0.2500 0.058(8) Uiso 0.096(7) d SP .
P2 P 0.0000 0.33198(4) 0.2500 0.0439(2) Uani 1 d S .
F21 F 0.07238(15) 0.33135(8) 0.16225(13) 0.0741(5) Uani 1 d . .
F22 F -0.10745(14) 0.33164(7) 0.16653(12) 0.0641(5) Uani 1 d . .
F23 F 0.0000 0.27063(9) 0.2500 0.0690(7) Uani 1 d S .
F24 F 0.0000 0.39293(9) 0.2500 0.0742(7) Uani 1 d S .
N001 N 0.7872(4) 0.10003(18) 0.0320(3) 0.1231(17) Uani 1 d . .
C001 C 0.6996(5) 0.08183(18) 0.0046(3) 0.0964(16) Uani 1 d . .
C002 C 0.5948(4) 0.0606(2) -0.0291(3) 0.1105(16) Uani 1 d . .
H02A H 0.5557 0.0575 0.0285 0.166 Uiso 1 calc R .
H02B H 0.6026 0.0266 -0.0584 0.166 Uiso 1 calc R .
H02C H 0.5537 0.0831 -0.0806 0.166 Uiso 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'
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'
Ni Ni 0.3393 1.1124 '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
N8 Ni1 N8 171.60(10) 2_655 . y
N8 Ni1 N14 77.79(7) 2_655 2_655 ?
N8 Ni1 N14 108.42(7) . 2_655 ?
N8 Ni1 N14 108.42(7) 2_655 . y
N8 Ni1 N14 77.79(7) . . y
N14 Ni1 N14 88.90(10) 2_655 . y
N8 Ni1 N1 77.95(7) 2_655 2_655 ?
N8 Ni1 N1 96.24(7) . 2_655 y
N14 Ni1 N1 155.19(7) 2_655 2_655 ?
N14 Ni1 N1 93.85(7) . 2_655 y
N8 Ni1 N1 96.24(7) 2_655 . ?
N8 Ni1 N1 77.95(7) . . y
N14 Ni1 N1 93.85(7) 2_655 . ?
N14 Ni1 N1 155.19(7) . . y
N1 Ni1 N1 93.88(9) 2_655 . y
C19 S1 C20 99.53(12) . . ?
C2 N1 C6 117.74(18) . . ?
C2 N1 Ni1 128.02(15) . . ?
C6 N1 Ni1 114.24(14) . . ?
N1 C2 C3 123.4(2) . . ?
C4 C3 C2 118.6(2) . . ?
C3 C4 C5 119.3(2) . . ?
C4 C5 C6 119.0(2) . . ?
N1 C6 C5 122.0(2) . . ?
N1 C6 C7 114.72(18) . . ?
C5 C6 C7 123.3(2) . . ?
N8 C7 C12 120.1(2) . . ?
N8 C7 C6 113.83(18) . . ?
C12 C7 C6 126.03(19) . . ?
C7 N8 C9 121.49(18) . . ?
C7 N8 Ni1 118.64(14) . . ?
C9 N8 Ni1 119.13(13) . . ?
N8 C9 C10 120.84(19) . . ?
N8 C9 C13 113.01(18) . . ?
C10 C9 C13 126.1(2) . . ?
C11 C10 C9 118.2(2) . . ?
C10 C11 C12 120.8(2) . . ?
C11 C12 C7 118.5(2) . . ?
N14 C13 C18 121.9(2) . . ?
N14 C13 C9 114.33(18) . . ?
C18 C13 C9 123.7(2) . . ?
C15 N14 C13 118.32(18) . . ?
C15 N14 Ni1 126.41(15) . . ?
C13 N14 Ni1 114.89(13) . . ?
N14 C15 C16 123.1(2) . . ?
C17 C16 C15 117.5(2) . . ?
C17 C16 C19 123.0(2) . . ?
C15 C16 C19 119.4(2) . . ?
C16 C17 C18 120.0(2) . . ?
C13 C18 C17 119.1(2) . . ?
C16 C19 S1 112.10(16) . . ?
C21 C20 S1 110.69(15) . . ?
C20 C21 C20 114.3(3) 2_655 . ?
F14B P1 F12B 78.7(10) . 2_655 ?
F14B P1 F12B 78.7(10) . . ?
F12B P1 F12B 157(2) 2_655 . ?
F14B P1 F13A 133.37(14) . 2_655 ?
F12B P1 F13A 54.8(10) 2_655 2_655 ?
F12B P1 F13A 147.6(11) . 2_655 ?
F14B P1 F13A 133.36(14) . . ?
F12B P1 F13A 147.6(11) 2_655 . ?
F12B P1 F13A 54.8(10) . . ?
F13A P1 F13A 93.3(3) 2_655 . ?
F14B P1 F12A 42.60(16) . . ?
F12B P1 F12A 121.1(11) 2_655 . ?
F12B P1 F12A 36.5(9) . . ?
F13A P1 F12A 175.9(2) 2_655 . ?
F13A P1 F12A 90.76(19) . . ?
F14B P1 F12A 42.60(16) . 2_655 ?
F12B P1 F12A 36.5(9) 2_655 2_655 ?
F12B P1 F12A 121.1(11) . 2_655 ?
F13A P1 F12A 90.77(19) 2_655 2_655 ?
F13A P1 F12A 175.9(2) . 2_655 ?
F12A P1 F12A 85.2(3) . 2_655 ?
F14B P1 F11 89.44(8) . . ?
F12B P1 F11 94.5(9) 2_655 . ?
F12B P1 F11 85.3(9) . . ?
F13A P1 F11 90.31(11) 2_655 . ?
F13A P1 F11 90.46(11) . . ?
F12A P1 F11 90.42(13) . . ?
F12A P1 F11 88.75(12) 2_655 . ?
F14B P1 F11 89.43(8) . 2_655 ?
F12B P1 F11 85.3(9) 2_655 2_655 ?
F12B P1 F11 94.5(9) . 2_655 ?
F13A P1 F11 90.47(11) 2_655 2_655 ?
F13A P1 F11 90.31(11) . 2_655 ?
F12A P1 F11 88.75(12) . 2_655 ?
F12A P1 F11 90.42(13) 2_655 2_655 ?
F11 P1 F11 178.87(16) . 2_655 ?
F14B P1 F13B 180.000(2) . . ?
F12B P1 F13B 101.3(10) 2_655 . ?
F12B P1 F13B 101.3(10) . . ?
F13A P1 F13B 46.63(14) 2_655 . ?
F13A P1 F13B 46.64(14) . . ?
F12A P1 F13B 137.40(16) . . ?
F12A P1 F13B 137.40(16) 2_655 . ?
F11 P1 F13B 90.56(8) . . ?
F11 P1 F13B 90.57(8) 2_655 . ?
F12B F12A F14B 119(2) . . ?
F12B F12A P1 60.4(13) . . ?
F14B F12A P1 59.2(14) . . ?
F13B F13A F12B 125.1(13) . . ?
F13B F13A P1 68.8(10) . . ?
F12B F13A P1 56.6(8) . . ?
F12A F12B F13A 150(2) . . ?
F12A F12B P1 83.1(14) . . ?
F13A F12B P1 68.6(11) . . ?
F12A F12B F14B 33.0(11) . . ?
F13A F12B F14B 119.2(14) . . ?
P1 F12B F14B 50.7(9) . . ?
F13A F13B F13A 129(2) 2_655 . ?
F13A F13B P1 64.6(10) 2_655 . ?
F13A F13B P1 64.6(10) . . ?
F12A F14B F12A 156(3) 2_655 . ?
F12A F14B P1 78.2(14) 2_655 . ?
F12A F14B P1 78.2(14) . . ?
F12A F14B F12B 128(2) 2_655 . ?
F12A F14B F12B 28.1(11) . . ?
P1 F14B F12B 50.6(9) . . ?
F12A F14B F12B 28.1(11) 2_655 2_655 ?
F12A F14B F12B 128(2) . 2_655 ?
P1 F14B F12B 50.6(9) . 2_655 ?
F12B F14B F12B 101.1(19) . 2_655 ?
F24 P2 F22 90.32(7) . 2 ?
F24 P2 F22 90.32(7) . . ?
F22 P2 F22 179.36(15) 2 . ?
F24 P2 F21 90.59(8) . 2 ?
F22 P2 F21 89.61(9) 2 2 ?
F22 P2 F21 90.38(9) . 2 ?
F24 P2 F21 90.59(8) . . ?
F22 P2 F21 90.38(9) 2 . ?
F22 P2 F21 89.61(9) . . ?
F21 P2 F21 178.83(16) 2 . ?
F24 P2 F23 180.0 . . ?
F22 P2 F23 89.68(7) 2 . ?
F22 P2 F23 89.68(7) . . ?
F21 P2 F23 89.41(8) 2 . ?
F21 P2 F23 89.41(8) . . ?
N001 C001 C002 179.3(5) . . ?
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
Ni1 N8 2.0031(17) 2_655 ?
Ni1 N8 2.0032(17) . y
Ni1 N14 2.1028(17) 2_655 ?
Ni1 N14 2.1029(17) . y
Ni1 N1 2.1124(17) 2_655 ?
Ni1 N1 2.1125(17) . y
S1 C19 1.817(3) . y
S1 C20 1.820(2) . y
N1 C2 1.340(3) . ?
N1 C6 1.350(3) . ?
C2 C3 1.372(3) . ?
C3 C4 1.373(3) . ?
C4 C5 1.381(4) . ?
C5 C6 1.384(3) . ?
C6 C7 1.482(3) . ?
C7 N8 1.341(3) . ?
C7 C12 1.393(3) . ?
N8 C9 1.344(3) . ?
C9 C10 1.383(3) . ?
C9 C13 1.491(3) . ?
C10 C11 1.382(3) . ?
C11 C12 1.382(3) . ?
C13 N14 1.353(3) . ?
C13 C18 1.377(3) . ?
N14 C15 1.344(3) . ?
C15 C16 1.394(3) . ?
C16 C17 1.380(3) . ?
C16 C19 1.506(3) . ?
C17 C18 1.386(3) . ?
C20 C21 1.533(3) . ?
C21 C20 1.533(3) 2_655 ?
P1 F14B 1.39(3) . ?
P1 F12B 1.39(2) 2_655 ?
P1 F12B 1.39(2) . ?
P1 F13A 1.553(2) 2_655 ?
P1 F13A 1.553(2) . ?
P1 F12A 1.589(3) . ?
P1 F12A 1.589(3) 2_655 ?
P1 F11 1.5900(16) . ?
P1 F11 1.5901(16) 2_655 ?
P1 F13B 1.60(2) . ?
F12A F12B 0.95(2) . ?
F12A F14B 1.099(7) . ?
F13A F13B 1.250(11) . ?
F13A F12B 1.36(2) . ?
F12B F14B 1.77(3) . ?
F13B F13A 1.250(11) 2_655 ?
F14B F12A 1.099(7) 2_655 ?
F14B F12B 1.77(3) 2_655 ?
P2 F24 1.585(3) . ?
P2 F22 1.5893(16) 2 ?
P2 F22 1.5894(16) . ?
P2 F21 1.5930(16) 2 ?
P2 F21 1.5930(16) . ?
P2 F23 1.595(2) . ?
N001 C001 1.187(7) . ?
C001 C002 1.414(7) . ?
