#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:39:32 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180048 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/42/7034241.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_7034241
loop_
_publ_author_name
'López-Banet, Luisa'
'Santana, M. Dolores'
'García, Gabriel'
'Pérez, José'
'García, Luís'
'Lezama, Luis'
'da Silva, Iván'
_publ_section_title
;
 Blocking and bridging ligands direct the structure and magnetic
 properties of dimers of pentacoordinate nickel(ii).
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6839
_journal_page_last               6847
_journal_paper_doi               10.1039/c5dt00181a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C26 H50 F12 N6 Ni2 O4 P2'
_chemical_formula_weight         918.08
_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
_audit_update_record
;
2015-02-20 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.6130(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.1736(4)
_cell_length_b                   15.1274(8)
_cell_length_c                   14.9948(8)
_cell_measurement_reflns_used    6670
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.7785
_cell_measurement_theta_min      2.693
_cell_volume                     1853.93(17)
_computing_data_collection       'Bruker SMART v5.625'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_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  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21309
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         28.22
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    1.203
_exptl_absorpt_correction_T_max  0.8994
_exptl_absorpt_correction_T_min  0.6851
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       latt
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.243
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4329
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.243
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0588
_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)+(0.0363P)²+3.7274P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1274
_reflns_number_gt                4026
_reflns_number_total             4329
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00181a2.cif
_cod_data_source_block           Comp5
_cod_depositor_comments
'Adding full bibliography for 7034237--7034241.cif.'
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7034241
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
Ni1 Ni 0.66962(5) 0.35594(3) 0.54659(3) 0.02086(13) Uani 1 1 d .
P1 P 0.42062(12) 0.55081(6) 0.78958(7) 0.0300(2) Uani 1 1 d .
F3 F 0.4691(3) 0.65173(16) 0.80648(17) 0.0468(6) Uani 1 1 d .
O2 O 0.4308(3) 0.39639(15) 0.53307(17) 0.0234(5) Uani 1 1 d .
F1 F 0.5065(3) 0.55414(15) 0.69440(15) 0.0399(6) Uani 1 1 d .
N1 N 0.9016(3) 0.3158(2) 0.5314(2) 0.0270(7) Uani 1 1 d .
O1 O 0.7104(3) 0.48262(16) 0.50529(18) 0.0281(6) Uani 1 1 d .
N2 N 0.5857(3) 0.23014(19) 0.5448(2) 0.0259(6) Uani 1 1 d .
H2 H 0.4745 0.2358 0.5325 0.031 Uiso 1 1 calc R
F6 F 0.2521(3) 0.57899(18) 0.7459(2) 0.0545(7) Uani 1 1 d .
F5 F 0.5910(3) 0.52033(18) 0.83438(18) 0.0517(7) Uani 1 1 d .
F4 F 0.3782(3) 0.44801(15) 0.77275(16) 0.0398(6) Uani 1 1 d .
F2 F 0.3373(4) 0.54581(18) 0.88522(18) 0.0587(8) Uani 1 1 d .
N3 N 0.6973(4) 0.3775(2) 0.6787(2) 0.0310(7) Uani 1 1 d .
H3 H 0.6094 0.4130 0.6947 0.037 Uiso 1 1 calc R
C1 C 0.9517(4) 0.2413(3) 0.5027(2) 0.0275(8) Uani 1 1 d .
C13 C 0.4189(4) 0.4753(2) 0.5082(2) 0.0211(7) Uani 1 1 d .
C10 C 1.1304(4) 0.2164(3) 0.4969(3) 0.0354(9) Uani 1 1 d .
H10A H 1.1981 0.2664 0.5165 0.053 Uiso 1 1 calc R
H10B H 1.1567 0.2014 0.4352 0.053 Uiso 1 1 calc R
H10C H 1.1524 0.1653 0.5355 0.053 Uiso 1 1 calc R
C2 C 0.8371(4) 0.1685(3) 0.4745(3) 0.0287(8) Uani 1 1 d .
H2A H 0.8492 0.1201 0.5184 0.034 Uiso 1 1 calc R
H2B H 0.8766 0.1455 0.4168 0.034 Uiso 1 1 calc R
C4 C 0.5927(5) 0.1780(2) 0.6284(3) 0.0320(8) Uani 1 1 d .
H4A H 0.7039 0.1531 0.6364 0.038 Uiso 1 1 calc R
H4B H 0.5146 0.1282 0.6241 0.038 Uiso 1 1 calc R
C11 C 0.6223(5) 0.2508(3) 0.3858(3) 0.0364(9) Uani 1 1 d .
H11A H 0.5046 0.2621 0.3798 0.055 Uiso 1 1 calc R
H11B H 0.6629 0.2247 0.3305 0.055 Uiso 1 1 calc R
H11C H 0.6796 0.3066 0.3975 0.055 Uiso 1 1 calc R
C9 C 1.0178(4) 0.3819(3) 0.5661(3) 0.0395(10) Uani 1 1 d .
H9A H 0.9951 0.4398 0.5378 0.047 Uiso 1 1 calc R
H9B H 1.1306 0.3642 0.5505 0.047 Uiso 1 1 calc R
C3 C 0.6533(4) 0.1868(2) 0.4634(3) 0.0291(8) Uani 1 1 d .
C12 C 0.5676(5) 0.0987(3) 0.4435(3) 0.0450(11) Uani 1 1 d .
H12A H 0.5875 0.0575 0.4929 0.068 Uiso 1 1 calc R
H12B H 0.6107 0.0736 0.3883 0.068 Uiso 1 1 calc R
H12C H 0.4496 0.1087 0.4366 0.068 Uiso 1 1 calc R
C5 C 0.5512(5) 0.2344(3) 0.7085(3) 0.0386(9) Uani 1 1 d .
H5A H 0.5263 0.1951 0.7593 0.046 Uiso 1 1 calc R
H5B H 0.4513 0.2690 0.6946 0.046 Uiso 1 1 calc R
C8 C 1.0051(5) 0.3908(3) 0.6664(3) 0.0447(11) Uani 1 1 d .
H8A H 1.0180 0.3314 0.6933 0.054 Uiso 1 1 calc R
H8B H 1.0974 0.4276 0.6880 0.054 Uiso 1 1 calc R
C6 C 0.6871(5) 0.2980(3) 0.7365(3) 0.0397(10) Uani 1 1 d .
H6A H 0.6684 0.3171 0.7987 0.048 Uiso 1 1 calc R
H6B H 0.7931 0.2664 0.7351 0.048 Uiso 1 1 calc R
C7 C 0.8474(5) 0.4307(3) 0.7000(3) 0.0429(11) Uani 1 1 d .
H7A H 0.8562 0.4378 0.7655 0.051 Uiso 1 1 calc R
H7B H 0.8343 0.4904 0.6737 0.051 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'
F F 0.0171 0.0103 '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'
Ni Ni 0.3393 1.1124 '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'
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 N3 93.69(13) . .
N1 Ni1 N2 91.96(12) . .
N3 Ni1 N2 101.52(13) . .
N1 Ni1 O1 95.30(11) . .
N3 Ni1 O1 97.40(12) . .
N2 Ni1 O1 159.24(12) . .
N1 Ni1 O2 167.81(12) . .
N3 Ni1 O2 98.35(12) . .
N2 Ni1 O2 87.56(10) . .
O1 Ni1 O2 81.27(9) . .
F6 P1 F2 90.37(18) . .
F6 P1 F3 91.23(16) . .
F2 P1 F3 90.58(14) . .
F6 P1 F1 90.62(15) . .
F2 P1 F1 178.81(17) . .
F3 P1 F1 90.06(13) . .
F6 P1 F5 178.95(16) . .
F2 P1 F5 89.25(17) . .
F3 P1 F5 89.76(15) . .
F1 P1 F5 89.75(15) . .
F6 P1 F4 90.59(14) . .
F2 P1 F4 90.10(14) . .
F3 P1 F4 178.05(16) . .
F1 P1 F4 89.22(13) . .
F5 P1 F4 88.43(14) . .
C13 O2 Ni1 112.6(2) . .
C1 N1 C9 120.8(3) . .
C1 N1 Ni1 127.8(3) . .
C9 N1 Ni1 111.2(2) . .
C13 O1 Ni1 112.8(2) 3_666 .
C4 N2 C3 116.5(3) . .
C4 N2 Ni1 118.7(2) . .
C3 N2 Ni1 107.1(2) . .
C6 N3 C7 111.2(3) . .
C6 N3 Ni1 115.8(2) . .
C7 N3 Ni1 112.3(3) . .
N1 C1 C2 122.7(3) . .
N1 C1 C10 123.6(3) . .
C2 C1 C10 113.7(3) . .
O1 C13 O2 126.6(3) 3_666 .
O1 C13 C13 117.1(4) 3_666 3_666
O2 C13 C13 116.3(3) . 3_666
C1 C2 C3 120.3(3) . .
N2 C4 C5 111.4(3) . .
N1 C9 C8 111.1(3) . .
N2 C3 C11 106.4(3) . .
N2 C3 C12 111.6(3) . .
C11 C3 C12 109.3(3) . .
N2 C3 C2 111.1(3) . .
C11 C3 C2 110.5(3) . .
C12 C3 C2 108.0(3) . .
C4 C5 C6 113.9(3) . .
C7 C8 C9 115.7(3) . .
N3 C6 C5 113.3(3) . .
N3 C7 C8 114.4(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 2.006(3) .
Ni1 N3 2.018(3) .
Ni1 N2 2.023(3) .
Ni1 O1 2.042(2) .
Ni1 O2 2.053(2) .
P1 F6 1.578(3) .
P1 F2 1.596(3) .
P1 F3 1.597(2) .
P1 F1 1.598(2) .
P1 F5 1.607(3) .
P1 F4 1.612(2) .
O2 C13 1.254(4) .
N1 C1 1.275(5) .
N1 C9 1.471(5) .
O1 C13 1.248(4) 3_666
N2 C4 1.481(5) .
N2 C3 1.497(5) .
N3 C6 1.485(5) .
N3 C7 1.499(5) .
C1 C2 1.503(5) .
C1 C10 1.512(5) .
C13 O1 1.248(4) 3_666
C13 C13 1.544(6) 3_666
C2 C3 1.535(5) .
C4 C5 1.515(6) .
C11 C3 1.532(5) .
C9 C8 1.515(7) .
C3 C12 1.534(5) .
C5 C6 1.525(6) .
C8 C7 1.514(6) .
