#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:09:59 +0100 (vie 25 de mar de 2016) $
#$Revision: 179742 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/38/7003822.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_7003822
loop_
_publ_author_name
'Majoumo-Mbé, F.'
'Kühl, O.'
'Lönnecke, P.'
'Silaghi-Dumitrescu, I.'
'Hey-Hawkins, E.'
_publ_section_title
;
 Bis(phosphanylamino)benzene ligands: a zinc(ii) complex and an unusual
 nickel(i) complex with a Dewar-benzene-type Ni2P2N2 backbone
;
_journal_issue                   23
_journal_name_full               'Dalton Transactions'
_journal_page_first              3107
_journal_page_last               3114
_journal_paper_doi               10.1039/b720004h
_journal_year                    2008
_chemical_formula_sum            'C66 H60 N6 Ni2 P4'
_chemical_formula_weight         1178.50
_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                101.889(2)
_cell_angle_beta                 100.363(2)
_cell_angle_gamma                107.307(2)
_cell_formula_units_Z            1
_cell_length_a                   9.5087(9)
_cell_length_b                   12.1620(12)
_cell_length_c                   13.8429(13)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.36
_cell_measurement_theta_min      2.84
_cell_volume                     1444.9(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP3 for Windows (L. J. Farrugia, 1997)'
_computing_publication_material  'WINGX (L.J. Farrugia,1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick,1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.904
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'ccd diffractometer (AXS Bruker)'
_diffrn_measurement_method       'ω 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  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15714
_diffrn_reflns_theta_full        29.02
_diffrn_reflns_theta_max         29.02
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.809
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             614
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         6949
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0384
_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)+(0.0540P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.1071
_reflns_number_gt                4687
_reflns_number_total             6949
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b720004h.txt
_cod_data_source_block           c936_fin
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7003822
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
Ni1 Ni 0.08808(4) 0.02608(3) 0.08263(2) 0.02636(10) Uani 1 1 d . . .
P1 P 0.23212(7) 0.06633(5) 0.23325(5) 0.02691(15) Uani 1 1 d . . .
P2 P 0.00639(7) 0.16181(5) -0.01843(5) 0.02657(15) Uani 1 1 d . . .
N1 N 0.3749(2) 0.19723(18) 0.25159(17) 0.0301(5) Uani 1 1 d . . .
N2 N 0.1405(2) 0.19006(17) 0.08556(16) 0.0304(5) Uani 1 1 d . . .
N3 N 0.7091(4) 0.2780(3) 0.3876(3) 0.0826(11) Uani 1 1 d . . .
C1 C 0.3451(3) -0.0219(2) 0.2717(2) 0.0316(6) Uani 1 1 d . . .
C2 C 0.3483(3) -0.0598(2) 0.3597(2) 0.0436(7) Uani 1 1 d . . .
H2 H 0.2928 -0.0372 0.4051 0.052 Uiso 1 1 calc R . .
C3 C 0.4339(4) -0.1315(3) 0.3810(3) 0.0591(10) Uani 1 1 d . . .
H3 H 0.4350 -0.1579 0.4403 0.071 Uiso 1 1 calc R . .
C4 C 0.5163(4) -0.1633(3) 0.3155(3) 0.0624(10) Uani 1 1 d . . .
H4 H 0.5743 -0.2110 0.3304 0.075 Uiso 1 1 calc R . .
C5 C 0.5150(3) -0.1261(3) 0.2281(3) 0.0553(9) Uani 1 1 d . . .
H5 H 0.5724 -0.1480 0.1838 0.066 Uiso 1 1 calc R . .
C6 C 0.4289(3) -0.0565(2) 0.2058(2) 0.0420(7) Uani 1 1 d . . .
H6 H 0.4267 -0.0322 0.1455 0.050 Uiso 1 1 calc R . .
C7 C 0.1397(3) 0.0931(2) 0.33615(19) 0.0312(6) Uani 1 1 d . . .
C8 C 0.2201(3) 0.1768(3) 0.4300(2) 0.0414(7) Uani 1 1 d . . .
H8 H 0.3255 0.2171 0.4427 0.050 Uiso 1 1 calc R . .
C9 C 0.1459(4) 0.2009(3) 0.5045(2) 0.0501(8) Uani 1 1 d . . .
H9 H 0.2012 0.2563 0.5681 0.060 Uiso 1 1 calc R . .
C10 C -0.0084(4) 0.1440(3) 0.4862(2) 0.0552(9) Uani 1 1 d . . .
H10 H -0.0585 0.1614 0.5369 0.066 Uiso 1 1 calc R . .
C11 C -0.0895(4) 0.0622(3) 0.3941(3) 0.0544(8) Uani 1 1 d . . .
H11 H -0.1951 0.0234 0.3818 0.065 Uiso 1 1 calc R . .
C12 C -0.0160(3) 0.0366(2) 0.3191(2) 0.0419(7) Uani 1 1 d . . .
H12 H -0.0722 -0.0197 0.2561 0.050 Uiso 1 1 calc R . .
C13 C 0.3467(3) 0.3022(2) 0.23934(19) 0.0287(5) Uani 1 1 d . . .
C14 C 0.2332(3) 0.2993(2) 0.15726(19) 0.0286(5) Uani 1 1 d . . .
C15 C 0.2199(3) 0.4092(2) 0.1492(2) 0.0330(6) Uani 1 1 d . . .
H15 H 0.1453 0.4098 0.0947 0.040 Uiso 1 1 calc R . .
C16 C 0.3142(3) 0.5174(2) 0.2197(2) 0.0381(6) Uani 1 1 d . . .
H16 H 0.3034 0.5899 0.2123 0.046 Uiso 1 1 calc R . .
C17 C 0.4230(3) 0.5178(2) 0.2999(2) 0.0400(7) Uani 1 1 d . . .
H17 H 0.4861 0.5904 0.3480 0.048 Uiso 1 1 calc R . .
C18 C 0.4394(3) 0.4115(2) 0.3097(2) 0.0362(6) Uani 1 1 d . . .
H18 H 0.5143 0.4124 0.3648 0.043 Uiso 1 1 calc R . .
C19 C -0.1397(3) 0.2216(2) 0.01518(19) 0.0300(6) Uani 1 1 d . . .
C20 C -0.2428(3) 0.1546(3) 0.0595(2) 0.0437(7) Uani 1 1 d . . .
H20 H -0.2361 0.0818 0.0690 0.052 Uiso 1 1 calc R . .
C21 C -0.3551(4) 0.1941(3) 0.0897(3) 0.0570(9) Uani 1 1 d . . .
H21 H -0.4235 0.1482 0.1197 0.068 Uiso 1 1 calc R . .
C22 C -0.3668(4) 0.3005(3) 0.0759(2) 0.0530(8) Uani 1 1 d . . .
H22 H -0.4427 0.3271 0.0967 0.064 Uiso 1 1 calc R . .
C23 C -0.2681(3) 0.3670(3) 0.0321(2) 0.0463(7) Uani 1 1 d . . .
H23 H -0.2765 0.4393 0.0225 0.056 Uiso 1 1 calc R . .
C24 C -0.1553(3) 0.3286(2) 0.0017(2) 0.0348(6) Uani 1 1 d . . .
H24 H -0.0881 0.3753 -0.0285 0.042 Uiso 1 1 calc R . .
C25 C 0.0883(3) 0.2497(2) -0.10094(19) 0.0290(5) Uani 1 1 d . . .
C26 C 0.2455(3) 0.2907(2) -0.0875(2) 0.0379(6) Uani 1 1 d . . .
H26 H 0.3086 0.2752 -0.0354 0.045 Uiso 1 1 calc R . .
C27 C 0.3096(4) 0.3541(3) -0.1506(2) 0.0488(8) Uani 1 1 d . . .
H27 H 0.4159 0.3813 -0.1411 0.059 Uiso 1 1 calc R . .
C28 C 0.2191(4) 0.3775(3) -0.2269(2) 0.0512(8) Uani 1 1 d . . .
H28 H 0.2634 0.4221 -0.2685 0.061 Uiso 1 1 calc R . .
C29 C 0.0634(4) 0.3354(2) -0.2425(2) 0.0469(8) Uani 1 1 d . . .
H29 H 0.0011 0.3502 -0.2955 0.056 Uiso 1 1 calc R . .
C30 C -0.0020(3) 0.2711(2) -0.17995(19) 0.0356(6) Uani 1 1 d . . .
H30 H -0.1086 0.2419 -0.1915 0.043 Uiso 1 1 calc R . .
C31 C 1.0790(5) 0.4450(4) 0.3963(3) 0.0851(13) Uani 1 1 d . . .
H31A H 1.0511 0.5160 0.4112 0.128 Uiso 1 1 calc R . .
H31B H 1.1680 0.4621 0.3693 0.128 Uiso 1 1 calc R . .
H31C H 1.1019 0.4215 0.4585 0.128 Uiso 1 1 calc R . .
C32 C 0.9491(4) 0.3451(4) 0.3191(3) 0.0760(11) Uani 1 1 d . . .
H32A H 0.9230 0.3713 0.2580 0.091 Uiso 1 1 calc R . .
H32B H 0.9820 0.2766 0.2991 0.091 Uiso 1 1 calc R . .
C33 C 0.8128(5) 0.3062(3) 0.3559(3) 0.0697(11) Uani 1 1 d . . .
H1N H 0.451(3) 0.212(2) 0.297(2) 0.041(9) 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
Ni Ni 0.3393 1.1124 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
N2 Ni1 P2 157.26(7) . 2 ?
N2 Ni1 P1 92.81(7) . . ?
P2 Ni1 P1 109.45(3) 2 . ?
N2 Ni1 Ni1 89.27(6) . 2 ?
P2 Ni1 Ni1 68.78(2) 2 2 ?
P1 Ni1 Ni1 176.14(3) . 2 ?
N2 Ni1 P2 39.59(6) . . ?
P2 Ni1 P2 118.86(2) 2 . ?
P1 Ni1 P2 131.56(3) . . ?
Ni1 Ni1 P2 50.078(18) 2 . ?
N1 P1 C1 99.11(11) . . ?
N1 P1 C7 105.38(11) . . ?
C1 P1 C7 104.53(12) . . ?
N1 P1 Ni1 106.62(8) . . ?
C1 P1 Ni1 124.46(9) . . ?
C7 P1 Ni1 114.30(9) . . ?
N2 P2 C19 109.01(11) . . ?
N2 P2 C25 108.26(11) . . ?
C19 P2 C25 104.48(11) . . ?
N2 P2 Ni1 108.03(7) . 2 ?
C19 P2 Ni1 110.69(8) . 2 ?
C25 P2 Ni1 116.16(8) . 2 ?
N2 P2 Ni1 47.44(7) . . ?
C19 P2 Ni1 118.41(9) . . ?
C25 P2 Ni1 135.23(8) . . ?
Ni1 P2 Ni1 61.14(2) 2 . ?
C13 N1 P1 122.23(18) . . ?
C14 N2 P2 130.47(17) . . ?
C14 N2 Ni1 135.35(18) . . ?
P2 N2 Ni1 92.97(9) . . ?
C2 C1 C6 118.7(2) . . ?
C2 C1 P1 124.1(2) . . ?
C6 C1 P1 117.1(2) . . ?
C1 C2 C3 120.1(3) . . ?
C4 C3 C2 119.9(3) . . ?
C3 C4 C5 120.8(3) . . ?
C4 C5 C6 119.6(3) . . ?
C5 C6 C1 120.8(3) . . ?
C12 C7 C8 118.5(2) . . ?
C12 C7 P1 120.0(2) . . ?
C8 C7 P1 121.4(2) . . ?
C9 C8 C7 120.4(3) . . ?
C10 C9 C8 120.3(3) . . ?
C11 C10 C9 120.2(3) . . ?
C10 C11 C12 120.0(3) . . ?
C7 C12 C11 120.7(3) . . ?
C18 C13 C14 120.1(2) . . ?
C18 C13 N1 118.0(2) . . ?
C14 C13 N1 121.9(2) . . ?
N2 C14 C15 122.2(2) . . ?
N2 C14 C13 120.4(2) . . ?
C15 C14 C13 117.4(2) . . ?
C16 C15 C14 121.8(3) . . ?
C17 C16 C15 119.7(2) . . ?
C16 C17 C18 119.9(2) . . ?
C17 C18 C13 121.1(3) . . ?
C20 C19 C24 117.4(2) . . ?
C20 C19 P2 116.7(2) . . ?
C24 C19 P2 125.9(2) . . ?
C21 C20 C19 120.8(3) . . ?
C22 C21 C20 120.3(3) . . ?
C23 C22 C21 119.9(3) . . ?
C22 C23 C24 120.4(3) . . ?
C23 C24 C19 121.2(3) . . ?
C30 C25 C26 118.6(2) . . ?
C30 C25 P2 122.1(2) . . ?
C26 C25 P2 119.3(2) . . ?
C27 C26 C25 120.3(3) . . ?
C28 C27 C26 120.5(3) . . ?
C27 C28 C29 119.8(3) . . ?
C28 C29 C30 120.2(3) . . ?
C25 C30 C29 120.6(3) . . ?
C33 C32 C31 113.6(3) . . ?
N3 C33 C32 177.8(4) . . ?
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 N2 1.8961(19) . ?
Ni1 P2 2.1150(7) 2 ?
Ni1 P1 2.1485(7) . ?
Ni1 Ni1 2.4152(6) 2 ?
Ni1 P2 2.5708(7) . ?
P1 N1 1.693(2) . ?
P1 C1 1.818(2) . ?
P1 C7 1.827(3) . ?
P2 N2 1.640(2) . ?
P2 C19 1.835(3) . ?
P2 C25 1.839(3) . ?
P2 Ni1 2.1150(7) 2 ?
N1 C13 1.417(3) . ?
N2 C14 1.404(3) . ?
N3 C33 1.141(5) . ?
C1 C2 1.387(4) . ?
C1 C6 1.396(4) . ?
C2 C3 1.397(4) . ?
C3 C4 1.370(5) . ?
C4 C5 1.374(5) . ?
C5 C6 1.383(4) . ?
C7 C12 1.386(4) . ?
C7 C8 1.394(4) . ?
C8 C9 1.381(4) . ?
C9 C10 1.373(4) . ?
C10 C11 1.370(4) . ?
C11 C12 1.386(4) . ?
C13 C18 1.397(3) . ?
C13 C14 1.406(3) . ?
C14 C15 1.405(3) . ?
C15 C16 1.394(3) . ?
C16 C17 1.373(4) . ?
C17 C18 1.379(4) . ?
C19 C20 1.396(4) . ?
C19 C24 1.398(3) . ?
C20 C21 1.390(4) . ?
C21 C22 1.379(5) . ?
C22 C23 1.363(4) . ?
C23 C24 1.388(4) . ?
C25 C30 1.383(4) . ?
C25 C26 1.392(4) . ?
C26 C27 1.385(4) . ?
C27 C28 1.371(4) . ?
C28 C29 1.374(4) . ?
C29 C30 1.389(4) . ?
C31 C32 1.497(5) . ?
C32 C33 1.460(6) . ?
