#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:07:09 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180026 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/20/7032026.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_7032026
loop_
_publ_author_name
'Dermitzaki, Despina'
'Raptopoulou, Catherine P.'
'Psycharis, Vassilis'
'Escuer, Albert'
'Perlepes, Spyros P.'
'Stamatatos, Theocharis C.'
_publ_section_title
;
 Unexpected metal ion-assisted transformations leading to unexplored
 bridging ligands in Ni(II) coordination chemistry: the case of PO3F(2-)
 group.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14520
_journal_page_last               14524
_journal_paper_doi               10.1039/c4dt02204a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C28 H36 F2 N8 Ni2 O12 P2'
_chemical_formula_weight         894.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 104.312(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.3339(1)
_cell_length_b                   12.9700(1)
_cell_length_c                   13.7335(2)
_cell_measurement_reflns_used    23287
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      72.03
_cell_measurement_theta_min      6.65
_cell_volume                     1783.58(3)
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            25502
_diffrn_reflns_theta_full        64.99
_diffrn_reflns_theta_max         64.99
_diffrn_reflns_theta_min         6.65
_exptl_absorpt_coefficient_mu    2.899
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         2914
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0350
_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)+(0.0472P)²+1.5911P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0901
_reflns_number_gt                2690
_reflns_number_total             2914
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02204a2.cif
_cod_data_source_block           comp3
_cod_depositor_comments
'Adding full bibliography for 7032024--7032027.cif.'
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7032026
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Ni Ni 0.44671(4) 0.07873(3) 0.31888(3) 0.01991(14) Uani 1 1 d .
O1 O 0.16089(19) 0.11510(15) 0.34837(15) 0.0335(4) Uani 1 1 d .
N1 N 0.2401(2) 0.06910(14) 0.29344(15) 0.0246(5) Uani 1 1 d .
N2 N 0.3927(2) -0.00622(14) 0.18574(14) 0.0247(5) Uani 1 1 d .
C1 C 0.0264(3) 0.0138(2) 0.1827(2) 0.0405(7) Uani 1 1 d .
H1A H 0.0004 -0.0570 0.1617 0.061 Uiso 1 1 calc R
H1B H -0.0077 0.0609 0.1265 0.061 Uiso 1 1 calc R
H1C H -0.0110 0.0326 0.2392 0.061 Uiso 1 1 calc R
C2 C 0.1753(3) 0.02118(18) 0.21437(18) 0.0278(6) Uani 1 1 d .
C3 C 0.2611(3) -0.02775(17) 0.15563(17) 0.0267(6) Uani 1 1 d .
C4 C 0.2109(3) -0.0934(2) 0.0754(2) 0.0373(7) Uani 1 1 d .
C5 C 0.2982(3) -0.1367(2) 0.0255(2) 0.0434(8) Uani 1 1 d .
C6 C 0.4320(3) -0.1141(2) 0.0554(2) 0.0376(7) Uani 1 1 d .
C7 C 0.4760(3) -0.04865(19) 0.13702(19) 0.0309(6) Uani 1 1 d .
O2 O 0.75707(17) 0.04308(14) 0.37311(14) 0.0304(4) Uani 1 1 d .
N3 N 0.6480(2) 0.09745(14) 0.31907(14) 0.0214(4) Uani 1 1 d .
N4 N 0.4431(2) 0.21277(14) 0.23310(14) 0.0212(4) Uani 1 1 d .
C8 C 0.8177(3) 0.2139(2) 0.2834(2) 0.0386(7) Uani 1 1 d .
H8A H 0.8785 0.1790 0.3398 0.058 Uiso 1 1 calc R
H8B H 0.8228 0.2886 0.2946 0.058 Uiso 1 1 calc R
H8C H 0.8432 0.1977 0.2210 0.058 Uiso 1 1 calc R
C9 C 0.6787(2) 0.17814(17) 0.27547(17) 0.0235(5) Uani 1 1 d .
C10 C 0.5632(2) 0.23749(17) 0.21694(17) 0.0222(5) Uani 1 1 d .
C11 C 0.5762(3) 0.31361(18) 0.1492(2) 0.0294(6) Uani 1 1 d .
C12 C 0.4625(3) 0.3651(2) 0.0962(2) 0.0334(6) Uani 1 1 d .
C13 C 0.3412(3) 0.34227(19) 0.1149(2) 0.0311(6) Uani 1 1 d .
C14 C 0.3356(3) 0.26550(18) 0.18400(19) 0.0263(6) Uani 1 1 d .
F F 0.48310(16) 0.23696(10) 0.60861(10) 0.0357(4) Uani 1 1 d .
P P 0.45350(6) 0.13401(4) 0.54433(4) 0.02192(17) Uani 1 1 d .
O3 O 0.48378(17) 0.16568(11) 0.44685(11) 0.0243(4) Uani 1 1 d .
O4 O 0.45556(17) -0.05618(12) 0.39470(12) 0.0253(4) Uani 1 1 d .
O5 O 0.30599(17) 0.11397(13) 0.53413(13) 0.0296(4) Uani 1 1 d .
O1W O 0.6568(3) 0.33300(19) 0.45295(19) 0.0666(7) Uani 1 1 d D
H1WA H 0.597(4) 0.276(3) 0.453(3) 0.112(17) Uiso 1 1 d D
H1WB H 0.714(4) 0.329(4) 0.517(2) 0.139 Uiso 1 1 d D
H1O H 0.204(4) 0.113(3) 0.405(3) 0.054(11) Uiso 1 1 d .
H2O H 0.731(3) -0.006(3) 0.405(3) 0.051(10) Uiso 1 1 d .
H4 H 0.118(3) -0.114(2) 0.060(2) 0.044(9) Uiso 1 1 d .
H5 H 0.267(3) -0.180(2) -0.025(2) 0.048(9) Uiso 1 1 d .
H6 H 0.498(3) -0.138(2) 0.025(2) 0.033(8) Uiso 1 1 d .
H7 H 0.573(3) -0.032(2) 0.1607(19) 0.026(7) Uiso 1 1 d .
H11 H 0.660(3) 0.331(2) 0.141(2) 0.028(7) Uiso 1 1 d .
H12 H 0.468(3) 0.419(2) 0.048(2) 0.036(8) Uiso 1 1 d .
H13 H 0.262(3) 0.376(2) 0.084(2) 0.032(7) Uiso 1 1 d .
H14 H 0.255(3) 0.249(2) 0.197(2) 0.029(7) Uiso 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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
O4 Ni O3 93.41(6) .
O4 Ni N1 87.05(7) .
O3 Ni N1 98.28(7) .
O4 Ni N2 87.86(7) .
O3 Ni N2 175.35(8) .
N1 Ni N2 77.30(8) .
O4 Ni N3 100.42(7) .
O3 Ni N3 87.70(7) .
N1 Ni N3 170.18(7) .
N2 Ni N3 96.47(8) .
O4 Ni N4 176.00(7) .
O3 Ni N4 89.95(6) .
N1 Ni N4 94.61(7) .
N2 Ni N4 88.95(7) .
N3 Ni N4 77.54(7) .
N1 O1 H1O 105(3) .
C2 N1 O1 114.6(2) .
C2 N1 Ni 117.99(18) .
O1 N1 Ni 127.28(15) .
C7 N2 C3 119.2(2) .
C7 N2 Ni 126.23(17) .
C3 N2 Ni 114.11(17) .
C2 C1 H1A 109.5 .
C2 C1 H1B 109.5 .
H1A C1 H1B 109.5 .
C2 C1 H1C 109.5 .
H1A C1 H1C 109.5 .
H1B C1 H1C 109.5 .
N1 C2 C3 114.2(2) .
N1 C2 C1 124.1(3) .
C3 C2 C1 121.7(2) .
N2 C3 C4 121.4(3) .
N2 C3 C2 116.0(2) .
C4 C3 C2 122.6(2) .
C5 C4 C3 118.8(3) .
C5 C4 H4 121.1(18) .
C3 C4 H4 119.7(18) .
C6 C5 C4 119.9(3) .
C6 C5 H5 121(2) .
C4 C5 H5 119(2) .
C5 C6 C7 118.4(3) .
C5 C6 H6 125.9(17) .
C7 C6 H6 115.7(18) .
N2 C7 C6 122.3(3) .
N2 C7 H7 118.0(15) .
C6 C7 H7 119.8(15) .
N3 O2 H2O 110(2) .
C9 N3 O2 113.9(2) .
C9 N3 Ni 116.97(16) .
O2 N3 Ni 128.34(15) .
C14 N4 C10 118.6(2) .
C14 N4 Ni 127.27(17) .
C10 N4 Ni 113.53(15) .
C9 C8 H8A 109.5 .
C9 C8 H8B 109.5 .
H8A C8 H8B 109.5 .
C9 C8 H8C 109.5 .
H8A C8 H8C 109.5 .
H8B C8 H8C 109.5 .
N3 C9 C10 114.8(2) .
N3 C9 C8 124.4(2) .
C10 C9 C8 120.8(2) .
N4 C10 C11 121.6(2) .
N4 C10 C9 115.9(2) .
C11 C10 C9 122.5(2) .
C10 C11 C12 119.0(3) .
C10 C11 H11 120.1(16) .
C12 C11 H11 120.8(16) .
C13 C12 C11 119.4(2) .
C13 C12 H12 119.3(17) .
C11 C12 H12 121.3(17) .
C12 C13 C14 118.5(2) .
C12 C13 H13 123.9(17) .
C14 C13 H13 117.5(17) .
N4 C14 C13 122.8(3) .
N4 C14 H14 117.8(17) .
C13 C14 H14 119.4(17) .
O4 P O3 116.39(10) 3_656
O4 P O5 114.57(9) 3_656
O3 P O5 112.91(10) .
O4 P F 104.45(9) 3_656
O3 P F 102.18(8) .
O5 P F 104.25(9) .
P O3 Ni 125.34(9) .
P O4 Ni 144.77(11) 3_656
H1WA O1W H1WB 103(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni O4 2.0266(16) .
Ni O3 2.0431(16) .
Ni N1 2.080(2) .
Ni N2 2.0892(19) .
Ni N3 2.094(2) .
Ni N4 2.0951(19) .
O1 N1 1.379(3) .
O1 H1O 0.80(4) .
N1 C2 1.286(3) .
N2 C7 1.333(3) .
N2 C3 1.349(3) .
C1 C2 1.495(4) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 C3 1.481(4) .
C3 C4 1.388(3) .
C4 C5 1.379(5) .
C4 H4 0.96(3) .
C5 C6 1.373(4) .
C5 H5 0.89(3) .
C6 C7 1.390(4) .
C6 H6 0.94(3) .
C7 H7 1.00(3) .
O2 N3 1.380(2) .
O2 H2O 0.85(3) .
N3 C9 1.284(3) .
N4 C14 1.336(3) .
N4 C10 1.353(3) .
C8 C9 1.487(4) .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 C10 1.479(3) .
C10 C11 1.385(3) .
C11 C12 1.390(4) .
C11 H11 0.93(3) .
C12 C13 1.372(4) .
C12 H12 0.97(3) .
C13 C14 1.386(4) .
C13 H13 0.93(3) .
C14 H14 0.92(3) .
F P 1.5882(14) .
P O4 1.4881(16) 3_656
P O3 1.5053(17) .
P O5 1.5184(18) .
O4 P 1.4881(16) 3_656
O1W H1WA 0.969(19) .
O1W H1WB 0.938(19) .
