#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/00/38/7003819.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_7003819
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            'C42 H50 N2 P2'
_chemical_formula_weight         644.78
_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                83.586(2)
_cell_angle_beta                 83.405(2)
_cell_angle_gamma                70.247(2)
_cell_formula_units_Z            2
_cell_length_a                   10.6118(12)
_cell_length_b                   12.6111(14)
_cell_length_c                   14.9209(17)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      3.44
_cell_volume                     1861.2(4)
_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 0.896
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type  'ccd diffractometer (AXS Bruker)'
_diffrn_measurement_method       ω-scans
_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  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19834
_diffrn_reflns_theta_full        28.93
_diffrn_reflns_theta_max         28.93
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         8817
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0428
_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)+(0.0675P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1196
_reflns_number_gt                5553
_reflns_number_total             8817
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b720004h.txt
_cod_data_source_block           c876_fin
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7003819
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
C1 C 0.34999(17) 0.10542(14) 0.28619(13) 0.0415(4) Uani 1 1 d . . .
C2 C 0.27182(18) 0.13225(15) 0.36832(13) 0.0458(4) Uani 1 1 d . . .
C3 C 0.2135(2) 0.05612(19) 0.41398(17) 0.0593(6) Uani 1 1 d . . .
C4 C 0.2322(2) -0.04745(19) 0.3836(2) 0.0702(7) Uani 1 1 d . . .
C5 C 0.3097(2) -0.07408(17) 0.3040(2) 0.0689(7) Uani 1 1 d . . .
C6 C 0.36586(19) 0.00101(15) 0.25208(15) 0.0528(5) Uani 1 1 d . . .
C7 C 0.60426(17) 0.13035(13) 0.20517(12) 0.0391(4) Uani 1 1 d . . .
C8 C 0.67614(18) 0.07773(14) 0.28047(12) 0.0437(4) Uani 1 1 d . . .
C9 C 0.8157(2) 0.03197(16) 0.26789(16) 0.0520(5) Uani 1 1 d . . .
C10 C 0.88623(19) 0.03574(16) 0.18528(16) 0.0561(5) Uani 1 1 d . . .
C11 C 0.8148(2) 0.08978(18) 0.11235(16) 0.0582(5) Uani 1 1 d . . .
C12 C 0.67560(19) 0.13695(16) 0.12059(13) 0.0499(5) Uani 1 1 d . . .
C13 C 0.67046(17) 0.52221(13) 0.36484(11) 0.0373(4) Uani 1 1 d . . .
C14 C 0.63448(18) 0.56024(14) 0.45219(12) 0.0423(4) Uani 1 1 d . . .
C15 C 0.7202(2) 0.51164(16) 0.52004(13) 0.0450(4) Uani 1 1 d . . .
C16 C 0.84037(19) 0.42615(15) 0.50561(12) 0.0449(4) Uani 1 1 d . . .
C17 C 0.87136(19) 0.38514(16) 0.42062(13) 0.0447(4) Uani 1 1 d . . .
C18 C 0.78970(17) 0.43045(14) 0.34992(11) 0.0400(4) Uani 1 1 d . . .
C19 C 0.66941(17) 0.63351(14) 0.18349(12) 0.0398(4) Uani 1 1 d . . .
C20 C 0.69017(19) 0.59902(16) 0.09443(12) 0.0475(4) Uani 1 1 d . . .
C21 C 0.7644(2) 0.6455(2) 0.02947(15) 0.0595(5) Uani 1 1 d . . .
C22 C 0.8186(2) 0.72570(19) 0.04675(15) 0.0607(6) Uani 1 1 d . . .
C23 C 0.79752(19) 0.75936(17) 0.13270(16) 0.0536(5) Uani 1 1 d . . .
C24 C 0.72480(17) 0.71593(14) 0.20141(13) 0.0435(4) Uani 1 1 d . . .
C25 C 0.32466(16) 0.42398(13) 0.22954(11) 0.0342(4) Uani 1 1 d . . .
C26 C 0.37258(16) 0.51550(13) 0.22429(11) 0.0347(4) Uani 1 1 d . . .
C27 C 0.2901(2) 0.62136(15) 0.19287(13) 0.0462(4) Uani 1 1 d . . .
C28 C 0.1633(2) 0.63674(17) 0.16861(14) 0.0525(5) Uani 1 1 d . . .
C29 C 0.1153(2) 0.54768(16) 0.17409(14) 0.0507(5) Uani 1 1 d . . .
C30 C 0.19662(17) 0.44140(15) 0.20540(12) 0.0416(4) Uani 1 1 d . . .
C31 C 0.2493(3) 0.2389(2) 0.41372(17) 0.0568(5) Uani 1 1 d . . .
C32 C 0.1695(3) -0.1299(2) 0.4359(2) 0.1124(12) Uani 1 1 d . . .
H32A H 0.1832 -0.1926 0.4006 0.169 Uiso 1 1 calc R . .
H32B H 0.0749 -0.0925 0.4484 0.169 Uiso 1 1 calc R . .
H32C H 0.2105 -0.1568 0.4918 0.169 Uiso 1 1 calc R . .
C33 C 0.4399(3) -0.0312(2) 0.1626(2) 0.0705(7) Uani 1 1 d . . .
C34 C 0.6112(3) 0.0683(2) 0.37436(15) 0.0609(6) Uani 1 1 d . . .
C35 C 1.0373(3) -0.0160(3) 0.1747(3) 0.0865(9) Uani 1 1 d . . .
C36 C 0.6063(3) 0.1969(3) 0.03679(18) 0.0800(8) Uani 1 1 d . . .
C37 C 0.5052(2) 0.6526(2) 0.47633(16) 0.0526(5) Uani 1 1 d . . .
C38 C 0.9350(3) 0.3805(2) 0.57939(17) 0.0597(6) Uani 1 1 d . . .
C39 C 0.8337(3) 0.3774(2) 0.26122(15) 0.0546(5) Uani 1 1 d . . .
C40 C 0.6366(3) 0.5135(2) 0.06374(16) 0.0633(6) Uani 1 1 d . . .
C41 C 0.8986(3) 0.7739(3) -0.02675(18) 0.1026(10) Uani 1 1 d . . .
H41A H 0.9132 0.8380 -0.0062 0.154 Uiso 1 1 calc R . .
H41B H 0.8499 0.7970 -0.0799 0.154 Uiso 1 1 calc R . .
H41C H 0.9836 0.7174 -0.0409 0.154 Uiso 1 1 calc R . .
C42 C 0.7060(3) 0.76016(19) 0.29331(17) 0.0564(5) Uani 1 1 d . . .
N1 N 0.40800(15) 0.31543(11) 0.25823(10) 0.0388(3) Uani 1 1 d . . .
N2 N 0.50189(15) 0.49678(13) 0.25019(10) 0.0390(3) Uani 1 1 d . . .
P1 P 0.42026(4) 0.19840(4) 0.20739(3) 0.03842(13) Uani 1 1 d . . .
P2 P 0.55657(5) 0.59998(4) 0.27763(3) 0.03850(13) Uani 1 1 d . . .
H1N H 0.4561(18) 0.3165(15) 0.2970(12) 0.043(5) Uiso 1 1 d . . .
H2N H 0.5514(19) 0.4379(16) 0.2401(13) 0.046(6) Uiso 1 1 d . . .
H3 H 0.161(2) 0.0774(18) 0.4716(16) 0.074(7) Uiso 1 1 d . . .
H5 H 0.327(2) -0.1433(19) 0.2729(14) 0.074(7) Uiso 1 1 d . . .
H9 H 0.863(2) -0.0044(17) 0.3159(14) 0.061(6) Uiso 1 1 d . . .
H11 H 0.860(2) 0.0958(17) 0.0543(15) 0.064(6) Uiso 1 1 d . . .
H15 H 0.6944(17) 0.5335(14) 0.5800(13) 0.046(5) Uiso 1 1 d . . .
H17 H 0.9505(19) 0.3215(15) 0.4106(12) 0.046(5) Uiso 1 1 d . . .
H21 H 0.776(2) 0.6178(16) -0.0276(14) 0.061(6) Uiso 1 1 d . . .
H23 H 0.8301(19) 0.8145(16) 0.1447(12) 0.052(5) Uiso 1 1 d . . .
H27 H 0.327(2) 0.6833(17) 0.1837(13) 0.064(6) Uiso 1 1 d . . .
H28 H 0.110(2) 0.7065(19) 0.1440(15) 0.070(6) Uiso 1 1 d . . .
H29 H 0.026(2) 0.5568(17) 0.1526(14) 0.070(6) Uiso 1 1 d . . .
H30 H 0.1636(17) 0.3791(15) 0.2092(11) 0.045(5) Uiso 1 1 d . . .
H31A H 0.197(2) 0.2360(16) 0.4686(15) 0.060(6) Uiso 1 1 d . . .
H31B H 0.333(2) 0.2451(18) 0.4286(15) 0.077(7) Uiso 1 1 d . . .
H31C H 0.207(2) 0.308(2) 0.3748(16) 0.084(8) Uiso 1 1 d . . .
H33A H 0.538(2) -0.0415(18) 0.1587(14) 0.074(7) Uiso 1 1 d . . .
H33B H 0.412(2) 0.0242(19) 0.1084(15) 0.072(7) Uiso 1 1 d . . .
H33C H 0.432(2) -0.106(2) 0.1457(17) 0.102(8) Uiso 1 1 d . . .
H34A H 0.670(3) 0.047(2) 0.4117(18) 0.092(9) Uiso 1 1 d . . .
H34B H 0.536(3) 0.132(2) 0.3915(17) 0.099(9) Uiso 1 1 d . . .
H34C H 0.565(3) 0.011(2) 0.3817(18) 0.106(10) Uiso 1 1 d . . .
H35A H 1.068(3) -0.084(3) 0.2045(19) 0.100(10) Uiso 1 1 d . . .
H35B H 1.073(3) -0.014(2) 0.108(2) 0.117(11) Uiso 1 1 d . . .
H35C H 1.077(3) 0.036(2) 0.192(2) 0.116(11) Uiso 1 1 d . . .
H36A H 0.546(3) 0.165(2) 0.0233(19) 0.102(11) Uiso 1 1 d . . .
H36B H 0.667(3) 0.198(2) -0.010(2) 0.114(11) Uiso 1 1 d . . .
H36C H 0.549(3) 0.282(3) 0.044(2) 0.132(12) Uiso 1 1 d . . .
H37A H 0.509(2) 0.722(2) 0.4508(15) 0.073(7) Uiso 1 1 d . . .
H37B H 0.427(2) 0.6396(17) 0.4549(14) 0.067(6) Uiso 1 1 d . . .
H37C H 0.485(2) 0.6493(17) 0.5389(16) 0.069(7) Uiso 1 1 d . . .
H38A H 0.986(3) 0.296(2) 0.5780(17) 0.098(9) Uiso 1 1 d . . .
H38B H 0.900(3) 0.374(3) 0.637(2) 0.132(12) Uiso 1 1 d . . .
H38C H 1.003(3) 0.410(2) 0.5795(18) 0.100(9) Uiso 1 1 d . . .
H39A H 0.824(2) 0.431(2) 0.2069(19) 0.094(8) Uiso 1 1 d . . .
H39B H 0.924(3) 0.326(2) 0.2597(16) 0.085(8) Uiso 1 1 d . . .
H39C H 0.781(3) 0.335(2) 0.2485(18) 0.099(9) Uiso 1 1 d . . .
H40A H 0.665(2) 0.5060(19) -0.0006(17) 0.080(7) Uiso 1 1 d . . .
H40B H 0.541(2) 0.5363(18) 0.0750(15) 0.072(7) Uiso 1 1 d . . .
H40C H 0.676(2) 0.437(2) 0.0920(15) 0.076(7) Uiso 1 1 d . . .
H42A H 0.751(2) 0.7073(17) 0.3343(14) 0.057(6) Uiso 1 1 d . . .
H42B H 0.608(2) 0.7851(18) 0.3180(15) 0.074(7) Uiso 1 1 d . . .
H42C H 0.739(2) 0.8237(18) 0.2895(14) 0.069(6) 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 0.0033 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'
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
_geom_angle_publ_flag
C2 C1 C6 118.48(17) . . ?
C2 C1 P1 127.43(13) . . ?
C6 C1 P1 113.63(15) . . ?
C3 C2 C1 119.62(19) . . ?
C3 C2 C31 116.2(2) . . ?
C1 C2 C31 124.19(17) . . ?
C4 C3 C2 122.6(2) . . ?
C5 C4 C3 117.7(2) . . ?
C5 C4 C32 120.8(2) . . ?
C3 C4 C32 121.4(3) . . ?
C4 C5 C6 122.7(2) . . ?
C5 C6 C1 118.8(2) . . ?
C5 C6 C33 119.2(2) . . ?
C1 C6 C33 122.07(19) . . ?
C12 C7 C8 118.88(16) . . ?
C12 C7 P1 115.56(13) . . ?
C8 C7 P1 125.51(14) . . ?
C9 C8 C7 118.59(18) . . ?
C9 C8 C34 117.78(18) . . ?
C7 C8 C34 123.63(17) . . ?
C10 C9 C8 123.05(19) . . ?
C9 C10 C11 117.77(19) . . ?
C9 C10 C35 121.2(2) . . ?
C11 C10 C35 121.0(2) . . ?
C10 C11 C12 121.8(2) . . ?
C11 C12 C7 119.84(18) . . ?
C11 C12 C36 117.9(2) . . ?
C7 C12 C36 122.26(19) . . ?
C14 C13 C18 118.77(16) . . ?
C14 C13 P2 116.07(13) . . ?
C18 C13 P2 125.16(13) . . ?
C15 C14 C13 119.56(17) . . ?
C15 C14 C37 117.64(17) . . ?
C13 C14 C37 122.81(17) . . ?
C16 C15 C14 122.49(17) . . ?
C15 C16 C17 117.43(17) . . ?
C15 C16 C38 120.97(18) . . ?
C17 C16 C38 121.59(19) . . ?
C16 C17 C18 122.65(18) . . ?
C17 C18 C13 118.92(16) . . ?
C17 C18 C39 117.50(17) . . ?
C13 C18 C39 123.58(17) . . ?
C20 C19 C24 117.87(16) . . ?
C20 C19 P2 127.48(13) . . ?
C24 C19 P2 113.99(13) . . ?
C21 C20 C19 119.03(18) . . ?
C21 C20 C40 116.35(18) . . ?
C19 C20 C40 124.61(18) . . ?
C22 C21 C20 123.2(2) . . ?
C23 C22 C21 117.55(19) . . ?
C23 C22 C41 121.4(2) . . ?
C21 C22 C41 121.1(2) . . ?
C22 C23 C24 122.41(19) . . ?
C23 C24 C19 119.91(18) . . ?
C23 C24 C42 118.03(17) . . ?
C19 C24 C42 122.06(17) . . ?
C30 C25 C26 119.61(15) . . ?
C30 C25 N1 120.91(15) . . ?
C26 C25 N1 119.48(14) . . ?
C27 C26 C25 118.48(15) . . ?
C27 C26 N2 122.58(15) . . ?
C25 C26 N2 118.94(14) . . ?
C28 C27 C26 120.98(17) . . ?
C29 C28 C27 120.89(18) . . ?
C28 C29 C30 118.74(18) . . ?
C25 C30 C29 121.28(17) . . ?
C25 N1 P1 122.63(12) . . ?
C26 N2 P2 124.22(12) . . ?
N1 P1 C1 109.66(8) . . ?
N1 P1 C7 98.12(7) . . ?
C1 P1 C7 105.13(8) . . ?
N2 P2 C13 100.78(7) . . ?
N2 P2 C19 109.72(8) . . ?
C13 P2 C19 103.96(8) . . ?
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
C1 C2 1.405(3) . ?
C1 C6 1.415(2) . ?
C1 P1 1.8425(18) . ?
C2 C3 1.388(3) . ?
C2 C31 1.508(3) . ?
C3 C4 1.374(3) . ?
C4 C5 1.370(4) . ?
C4 C32 1.517(3) . ?
C5 C6 1.401(3) . ?
C6 C33 1.493(3) . ?
C7 C12 1.404(3) . ?
C7 C8 1.404(2) . ?
C7 P1 1.8463(18) . ?
C8 C9 1.394(3) . ?
C8 C34 1.499(3) . ?
C9 C10 1.372(3) . ?
C10 C11 1.378(3) . ?
C10 C35 1.509(3) . ?
C11 C12 1.390(3) . ?
C12 C36 1.516(3) . ?
C13 C14 1.406(2) . ?
C13 C18 1.412(2) . ?
C13 P2 1.8414(17) . ?
C14 C15 1.387(3) . ?
C14 C37 1.506(3) . ?
C15 C16 1.377(3) . ?
C16 C17 1.385(3) . ?
C16 C38 1.508(3) . ?
C17 C18 1.390(2) . ?
C18 C39 1.504(3) . ?
C19 C20 1.414(2) . ?
C19 C24 1.417(2) . ?
C19 P2 1.8463(18) . ?
C20 C21 1.383(3) . ?
C20 C40 1.510(3) . ?
C21 C22 1.380(3) . ?
C22 C23 1.366(3) . ?
C22 C41 1.510(3) . ?
C23 C24 1.387(3) . ?
C24 C42 1.505(3) . ?
C25 C30 1.385(2) . ?
C25 C26 1.402(2) . ?
C25 N1 1.406(2) . ?
C26 C27 1.390(2) . ?
C26 N2 1.404(2) . ?
C27 C28 1.378(3) . ?
C28 C29 1.373(3) . ?
C29 C30 1.389(3) . ?
N1 P1 1.6937(14) . ?
N2 P2 1.6978(15) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30652652
