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#$Date: 2016-03-22 12:30:20 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178952 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/81/4118105.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_4118105
loop_
_publ_author_name
'Ashley M. Wright'
'Guang Wu'
'Trevor W. Hayton'
_publ_section_title
;
 Formation of N2O from a Nickel Nitrosyl: Isolation of the cis-[N2O2]2-
 Intermediate
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9930
_journal_page_last               9933
_journal_paper_doi               10.1021/ja304204q
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C22 H20 Cl3 F6 N5 Ni O P'
_chemical_formula_weight         680.46
_chemical_name_systematic
; 
bis(bipyridine) nitrosyl nickel hexafluorophosphate
;
_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                91.115(2)
_cell_angle_beta                 102.721(2)
_cell_angle_gamma                107.306(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1746(12)
_cell_length_b                   12.0587(16)
_cell_length_c                   12.7075(16)
_cell_measurement_temperature    150(2)
_cell_volume                     1303.8(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD detector'
_diffrn_measurement_method       'Omega scan'
_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  0.0990
_diffrn_reflns_av_sigmaI/netI    0.0837
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11064
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    1.184
_exptl_absorpt_correction_T_max  0.7177
_exptl_absorpt_correction_T_min  0.6488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_description       block
_exptl_crystal_F_000             686
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0583P)²+0.3000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1322
_reflns_number_gt                4034
_reflns_number_total             5081
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja304204q_si_001_3.cif
_cod_data_source_block           complex_2
_cod_database_code               4118105
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
Ni1 Ni 0.48326(4) 0.47673(3) 0.22600(3) 0.02192(14) Uani 1 1 d .
P1 P 0.58807(10) 0.04551(7) 0.27802(8) 0.0301(2) Uani 1 1 d .
F5 F 0.6664(3) 0.17837(19) 0.3238(2) 0.0645(8) Uani 1 1 d .
F3 F 0.5516(3) 0.0122(2) 0.39306(18) 0.0477(6) Uani 1 1 d .
Cl1 Cl 0.09225(11) 0.71997(8) 0.34669(8) 0.0449(3) Uani 1 1 d .
F1 F 0.4221(3) 0.0693(2) 0.2439(2) 0.0581(7) Uani 1 1 d .
F2 F 0.5076(4) -0.0870(2) 0.2337(2) 0.0788(9) Uani 1 1 d .
F4 F 0.7533(3) 0.0231(2) 0.3146(3) 0.0765(9) Uani 1 1 d .
F6 F 0.6260(4) 0.0799(3) 0.1656(2) 0.0741(9) Uani 1 1 d .
Cl2 Cl 0.05744(13) 0.95135(9) 0.35801(10) 0.0567(3) Uani 1 1 d .
N5 N 0.4088(3) 0.3665(2) 0.0855(2) 0.0252(6) Uani 1 1 d .
N1 N 0.6658(3) 0.4498(2) 0.2508(2) 0.0258(6) Uani 1 1 d .
N4 N 0.3433(3) 0.5589(2) 0.1202(2) 0.0260(6) Uani 1 1 d .
N2 N 0.5321(3) 0.5939(2) 0.3503(2) 0.0229(6) Uani 1 1 d .
N3 N 0.2943(3) 0.4038(2) 0.2925(2) 0.0242(6) Uani 1 1 d .
C9 C 0.0492(4) 0.2674(3) 0.3023(3) 0.0339(8) Uani 1 1 d .
H9 H -0.0281 0.1963 0.2781 0.041 Uiso 1 1 calc R
C18 C 0.2819(4) 0.2150(3) -0.1006(3) 0.0369(8) Uani 1 1 d .
H18 H 0.2389 0.1640 -0.1631 0.044 Uiso 1 1 calc R
C1 C 0.6593(4) 0.6902(3) 0.3749(3) 0.0262(7) Uani 1 1 d .
H1 H 0.7365 0.6991 0.3362 0.031 Uiso 1 1 calc R
C19 C 0.3910(4) 0.1935(3) -0.0177(3) 0.0359(8) Uani 1 1 d .
H19 H 0.4233 0.1279 -0.0232 0.043 Uiso 1 1 calc R
C13 C 0.1482(4) 0.6468(3) -0.0291(3) 0.0400(9) Uani 1 1 d .
H13 H 0.0827 0.6766 -0.0792 0.048 Uiso 1 1 calc R
C21 C 0.1905(5) 0.8714(3) 0.3788(4) 0.0530(11) Uani 1 1 d .
H21A H 0.2488 0.8854 0.4540 0.064 Uiso 1 1 calc R
H21B H 0.2650 0.8975 0.3340 0.064 Uiso 1 1 calc R
C4 C 0.4353(4) 0.6623(3) 0.4898(3) 0.0279(7) Uani 1 1 d .
H4 H 0.3583 0.6510 0.5289 0.033 Uiso 1 1 calc R
C14 C 0.1681(4) 0.5413(3) -0.0535(3) 0.0355(8) Uani 1 1 d .
H14 H 0.1155 0.4986 -0.1198 0.043 Uiso 1 1 calc R
C10 C 0.1783(4) 0.3024(3) 0.2589(3) 0.0302(7) Uani 1 1 d .
H10 H 0.1859 0.2541 0.2038 0.036 Uiso 1 1 calc R
C17 C 0.2363(4) 0.3135(3) -0.0902(3) 0.0355(8) Uani 1 1 d .
H17 H 0.1621 0.3291 -0.1457 0.043 Uiso 1 1 calc R
C6 C 0.2840(3) 0.4734(3) 0.3730(2) 0.0236(6) Uani 1 1 d .
C7 C 0.1560(4) 0.4448(3) 0.4199(3) 0.0300(7) Uani 1 1 d .
H7 H 0.1498 0.4941 0.4748 0.036 Uiso 1 1 calc R
C15 C 0.2682(3) 0.4996(3) 0.0228(3) 0.0257(7) Uani 1 1 d .
C16 C 0.3025(4) 0.3889(3) 0.0037(3) 0.0268(7) Uani 1 1 d .
C2 C 0.6793(4) 0.7757(3) 0.4548(3) 0.0292(7) Uani 1 1 d .
H2 H 0.7670 0.8418 0.4687 0.035 Uiso 1 1 calc R
O1 O 0.7845(3) 0.4958(2) 0.3193(2) 0.0361(6) Uani 1 1 d .
C3 C 0.5669(4) 0.7617(3) 0.5140(3) 0.0318(8) Uani 1 1 d .
H3 H 0.5786 0.8177 0.5693 0.038 Uiso 1 1 calc R
C20 C 0.4518(4) 0.2710(3) 0.0739(3) 0.0300(7) Uani 1 1 d .
H20 H 0.5258 0.2564 0.1301 0.036 Uiso 1 1 calc R
C11 C 0.3217(4) 0.6614(3) 0.1426(3) 0.0314(7) Uani 1 1 d .
H11 H 0.3735 0.7025 0.2097 0.038 Uiso 1 1 calc R
C8 C 0.0367(4) 0.3395(3) 0.3820(3) 0.0338(8) Uani 1 1 d .
H8 H -0.0512 0.3185 0.4111 0.041 Uiso 1 1 calc R
C12 C 0.2263(4) 0.7078(3) 0.0702(3) 0.0395(8) Uani 1 1 d .
H12 H 0.2145 0.7793 0.0879 0.047 Uiso 1 1 calc R
C5 C 0.4210(3) 0.5812(2) 0.4074(2) 0.0220(6) Uani 1 1 d .
Cl3 Cl 0.93670(14) 0.07283(9) 1.05782(10) 0.0579(3) Uani 1 1 d .
C22 C 0.9251(10) 0.0092(7) 0.9301(7) 0.131(3) Uani 1 1 d .
H22A H 0.9490 0.0694 0.8814 0.158 Uiso 1 1 calc R
H22B H 0.8193 -0.0422 0.9002 0.158 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'
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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
N1 Ni1 N2 97.99(11) . .
N1 Ni1 N5 89.60(11) . .
N2 Ni1 N5 171.55(10) . .
N1 Ni1 N3 128.45(11) . .
N2 Ni1 N3 80.32(10) . .
N5 Ni1 N3 97.89(10) . .
N1 Ni1 N4 142.06(11) . .
N2 Ni1 N4 94.19(10) . .
N5 Ni1 N4 77.49(10) . .
N3 Ni1 N4 88.94(10) . .
F6 P1 F2 92.02(17) . .
F6 P1 F5 88.86(16) . .
F2 P1 F5 178.88(18) . .
F6 P1 F4 89.47(16) . .
F2 P1 F4 90.30(17) . .
F5 P1 F4 90.40(16) . .
F6 P1 F1 91.53(15) . .
F2 P1 F1 90.48(16) . .
F5 P1 F1 88.82(15) . .
F4 P1 F1 178.72(18) . .
F6 P1 F3 179.16(17) . .
F2 P1 F3 88.74(15) . .
F5 P1 F3 90.38(14) . .
F4 P1 F3 90.17(14) . .
F1 P1 F3 88.82(13) . .
C20 N5 C16 118.9(3) . .
C20 N5 Ni1 123.8(2) . .
C16 N5 Ni1 117.2(2) . .
O1 N1 Ni1 129.5(2) . .
C11 N4 C15 118.5(3) . .
C11 N4 Ni1 126.1(2) . .
C15 N4 Ni1 115.4(2) . .
C5 N2 C1 118.4(3) . .
C5 N2 Ni1 116.41(19) . .
C1 N2 Ni1 124.9(2) . .
C6 N3 C10 118.6(3) . .
C6 N3 Ni1 113.55(19) . .
C10 N3 Ni1 127.6(2) . .
C8 C9 C10 118.5(3) . .
C8 C9 H9 120.7 . .
C10 C9 H9 120.7 . .
C19 C18 C17 119.4(3) . .
C19 C18 H18 120.3 . .
C17 C18 H18 120.3 . .
N2 C1 C2 122.7(3) . .
N2 C1 H1 118.7 . .
C2 C1 H1 118.7 . .
C18 C19 C20 118.7(3) . .
C18 C19 H19 120.7 . .
C20 C19 H19 120.7 . .
C14 C13 C12 119.4(3) . .
C14 C13 H13 120.3 . .
C12 C13 H13 120.3 . .
Cl2 C21 Cl1 111.2(2) . .
Cl2 C21 H21A 109.4 . .
Cl1 C21 H21A 109.4 . .
Cl2 C21 H21B 109.4 . .
Cl1 C21 H21B 109.4 . .
H21A C21 H21B 108.0 . .
C5 C4 C3 119.2(3) . .
C5 C4 H4 120.4 . .
C3 C4 H4 120.4 . .
C13 C14 C15 118.9(3) . .
C13 C14 H14 120.5 . .
C15 C14 H14 120.5 . .
N3 C10 C9 122.9(3) . .
N3 C10 H10 118.6 . .
C9 C10 H10 118.6 . .
C18 C17 C16 119.4(3) . .
C18 C17 H17 120.3 . .
C16 C17 H17 120.3 . .
N3 C6 C7 121.9(3) . .
N3 C6 C5 114.5(3) . .
C7 C6 C5 123.5(3) . .
C6 C7 C8 118.0(3) . .
C6 C7 H7 121.0 . .
C8 C7 H7 121.0 . .
N4 C15 C14 121.6(3) . .
N4 C15 C16 114.9(3) . .
C14 C15 C16 123.5(3) . .
N5 C16 C17 120.9(3) . .
N5 C16 C15 114.6(3) . .
C17 C16 C15 124.5(3) . .
C1 C2 C3 118.9(3) . .
C1 C2 H2 120.6 . .
C3 C2 H2 120.6 . .
C2 C3 C4 119.0(3) . .
C2 C3 H3 120.5 . .
C4 C3 H3 120.5 . .
N5 C20 C19 122.8(3) . .
N5 C20 H20 118.6 . .
C19 C20 H20 118.6 . .
N4 C11 C12 122.6(3) . .
N4 C11 H11 118.7 . .
C12 C11 H11 118.7 . .
C9 C8 C7 120.1(3) . .
C9 C8 H8 119.9 . .
C7 C8 H8 119.9 . .
C11 C12 C13 119.0(4) . .
C11 C12 H12 120.5 . .
C13 C12 H12 120.5 . .
N2 C5 C4 121.9(3) . .
N2 C5 C6 114.4(3) . .
C4 C5 C6 123.8(3) . .
C22 Cl3 C22 70.5(4) . 2_757
Cl3 C22 Cl3 109.5(4) . 2_757
Cl3 C22 H22A 109.8 . .
Cl3 C22 H22A 109.8 2_757 .
Cl3 C22 H22B 109.8 . .
Cl3 C22 H22B 109.8 2_757 .
H22A C22 H22B 108.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 1.762(3) .
Ni1 N2 1.979(3) .
Ni1 N5 2.062(3) .
Ni1 N3 2.064(3) .
Ni1 N4 2.118(3) .
P1 F6 1.578(3) .
P1 F2 1.580(2) .
P1 F5 1.586(2) .
P1 F4 1.589(3) .
P1 F1 1.601(2) .
P1 F3 1.603(2) .
Cl1 C21 1.773(4) .
Cl2 C21 1.749(4) .
N5 C20 1.338(4) .
N5 C16 1.351(4) .
N1 O1 1.207(3) .
N4 C11 1.343(4) .
N4 C15 1.348(4) .
N2 C5 1.351(4) .
N2 C1 1.352(4) .
N3 C6 1.347(4) .
N3 C10 1.348(4) .
C9 C8 1.367(5) .
C9 C10 1.373(5) .
C9 H9 0.9300 .
C18 C19 1.371(5) .
C18 C17 1.385(5) .
C18 H18 0.9300 .
C1 C2 1.376(5) .
C1 H1 0.9300 .
C19 C20 1.379(5) .
C19 H19 0.9300 .
C13 C14 1.376(5) .
C13 C12 1.378(5) .
C13 H13 0.9300 .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C4 C5 1.376(4) .
C4 C3 1.397(4) .
C4 H4 0.9300 .
C14 C15 1.392(5) .
C14 H14 0.9300 .
C10 H10 0.9300 .
C17 C16 1.389(4) .
C17 H17 0.9300 .
C6 C7 1.388(5) .
C6 C5 1.491(4) .
C7 C8 1.400(5) .
C7 H7 0.9300 .
C15 C16 1.486(5) .
C2 C3 1.378(5) .
C2 H2 0.9300 .
C3 H3 0.9300 .
C20 H20 0.9300 .
C11 C12 1.372(5) .
C11 H11 0.9300 .
C8 H8 0.9300 .
C12 H12 0.9300 .
Cl3 C22 1.750(9) .
Cl3 C22 1.810(9) 2_757
C22 Cl3 1.810(9) 2_757
C22 H22A 0.9700 .
C22 H22B 0.9700 .
