#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:58:42 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179771 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/67/7006778.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_7006778
loop_
_publ_author_name
'Bai, Guangcai'
'Wei, Pingrong'
'Das, Anjan K.'
'Stephan, Douglas W.'
_publ_section_title
;
 P-H and P-P bond activation by Ni(I) and Fe(I)
 beta-diketiminato-complexes.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1141
_journal_page_last               1146
_journal_paper_doi               10.1039/b513892b
_journal_year                    2006
_chemical_formula_sum            'C41 H52 N2 Ni P'
_chemical_formula_weight         662.53
_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                 101.689(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3110(16)
_cell_length_b                   20.471(2)
_cell_length_c                   14.5076(17)
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     3871.2(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0770
_diffrn_reflns_av_sigmaI/netI    0.0625
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            36847
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.571
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.865586
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1420
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         6799
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1294
_refine_ls_R_factor_gt           0.0649
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1014P)²+3.7878P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1504
_refine_ls_wR_factor_ref         0.1950
_reflns_number_gt                3732
_reflns_number_total             6799
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b513892b.txt
_cod_data_source_block           (NacNac)Ni(PHPh2)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7006778
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 1.02268(5) 0.79345(3) 0.81040(4) 0.0609(3) Uani 1 1 d . . .
P1 P 0.92289(14) 0.73913(8) 0.69849(12) 0.0647(5) Uani 0.86 1 d PD . .
H30A H 0.8313 0.7336 0.7062 0.091(19) Uiso 0.86 1 d P . .
P1A P 1.0205(11) 0.7390(5) 0.6928(7) 0.091(4) Uani 0.14 1 d PD . .
N1 N 0.9981(3) 0.77311(18) 0.9330(3) 0.0555(10) Uani 1 1 d . . .
N2 N 1.1106(3) 0.86517(18) 0.8461(3) 0.0589(10) Uani 1 1 d . . .
C1 C 0.9187(4) 0.7262(2) 0.9369(3) 0.0588(13) Uani 1 1 d . . .
C2 C 0.9429(4) 0.6603(2) 0.9543(4) 0.0682(14) Uani 1 1 d . . .
C3 C 0.8615(6) 0.6161(3) 0.9469(4) 0.0889(18) Uani 1 1 d . . .
H3A H 0.8754 0.5718 0.9565 0.107 Uiso 1 1 calc R . .
C4 C 0.7625(5) 0.6368(4) 0.9260(5) 0.098(2) Uani 1 1 d . . .
H4A H 0.7095 0.6066 0.9215 0.118 Uiso 1 1 calc R . .
C5 C 0.7403(5) 0.7015(4) 0.9114(4) 0.0875(18) Uani 1 1 d . . .
H5A H 0.6721 0.7147 0.8980 0.105 Uiso 1 1 calc R . .
C6 C 0.8165(4) 0.7478(3) 0.9161(4) 0.0695(14) Uani 1 1 d . . .
C7 C 1.0530(5) 0.6365(3) 0.9819(5) 0.0886(18) Uani 1 1 d . . .
H7A H 1.0978 0.6749 0.9873 0.106 Uiso 1 1 calc R . .
C8 C 1.0819(6) 0.5918(4) 0.9076(6) 0.133(3) Uani 1 1 d . . .
H8A H 1.0688 0.6136 0.8478 0.199 Uiso 1 1 calc R . .
H8B H 1.0417 0.5525 0.9033 0.199 Uiso 1 1 calc R . .
H8C H 1.1534 0.5809 0.9249 0.199 Uiso 1 1 calc R . .
C9 C 1.0742(7) 0.6017(4) 1.0771(6) 0.146(3) Uani 1 1 d . . .
H9A H 1.0561 0.6299 1.1240 0.219 Uiso 1 1 calc R . .
H9B H 1.1457 0.5908 1.0942 0.219 Uiso 1 1 calc R . .
H9C H 1.0339 0.5624 1.0728 0.219 Uiso 1 1 calc R . .
C10 C 0.7898(4) 0.8188(3) 0.9023(5) 0.0890(18) Uani 1 1 d . . .
H10A H 0.8526 0.8422 0.8971 0.107 Uiso 1 1 calc R . .
C11 C 0.7102(7) 0.8335(4) 0.8144(6) 0.168(4) Uani 1 1 d . . .
H11A H 0.7321 0.8155 0.7606 0.252 Uiso 1 1 calc R . .
H11B H 0.7023 0.8799 0.8070 0.252 Uiso 1 1 calc R . .
H11C H 0.6458 0.8143 0.8199 0.252 Uiso 1 1 calc R . .
C12 C 0.7513(10) 0.8478(4) 0.9829(6) 0.195(5) Uani 1 1 d . . .
H12A H 0.7998 0.8395 1.0404 0.293 Uiso 1 1 calc R . .
H12B H 0.6865 0.8284 0.9866 0.293 Uiso 1 1 calc R . .
H12C H 0.7428 0.8940 0.9738 0.293 Uiso 1 1 calc R . .
C13 C 1.0229(5) 0.7847(3) 1.1055(4) 0.096(2) Uani 1 1 d . . .
H13A H 0.9580 0.8027 1.1118 0.143 Uiso 1 1 calc R . .
H13B H 1.0760 0.8015 1.1547 0.143 Uiso 1 1 calc R . .
H13C H 1.0207 0.7380 1.1101 0.143 Uiso 1 1 calc R . .
C14 C 1.0450(4) 0.8036(2) 1.0113(4) 0.0629(13) Uani 1 1 d . . .
C15 C 1.1142(4) 0.8541(3) 1.0104(4) 0.0692(14) Uani 1 1 d . . .
H15A H 1.1460 0.8698 1.0693 0.083 Uiso 1 1 calc R . .
C16 C 1.1430(4) 0.8848(2) 0.9334(4) 0.0663(14) Uani 1 1 d . . .
C17 C 1.2121(6) 0.9440(3) 0.9542(5) 0.114(3) Uani 1 1 d . . .
H17A H 1.2809 0.9320 0.9504 0.172 Uiso 1 1 calc R . .
H17B H 1.2112 0.9597 1.0163 0.172 Uiso 1 1 calc R . .
H17C H 1.1881 0.9776 0.9090 0.172 Uiso 1 1 calc R . .
C18 C 1.1335(4) 0.9021(2) 0.7692(4) 0.0656(14) Uani 1 1 d . . .
C19 C 1.2224(5) 0.8872(3) 0.7349(4) 0.0768(16) Uani 1 1 d . . .
C20 C 1.2410(6) 0.9237(4) 0.6593(5) 0.105(2) Uani 1 1 d . . .
H20A H 1.2995 0.9150 0.6357 0.126 Uiso 1 1 calc R . .
C21 C 1.1771(8) 0.9711(4) 0.6193(5) 0.120(3) Uani 1 1 d . . .
H21A H 1.1926 0.9950 0.5694 0.144 Uiso 1 1 calc R . .
C22 C 1.0881(7) 0.9846(3) 0.6518(5) 0.111(2) Uani 1 1 d . . .
H22A H 1.0435 1.0168 0.6226 0.133 Uiso 1 1 calc R . .
C23 C 1.0655(5) 0.9504(3) 0.7275(4) 0.0836(17) Uani 1 1 d . . .
C24 C 1.2920(4) 0.8325(3) 0.7741(5) 0.0930(19) Uani 1 1 d . . .
H24A H 1.2670 0.8146 0.8279 0.112 Uiso 1 1 calc R . .
C25 C 1.2864(8) 0.7784(4) 0.7019(6) 0.158(4) Uani 1 1 d . . .
H25A H 1.2163 0.7655 0.6804 0.238 Uiso 1 1 calc R . .
H25B H 1.3257 0.7416 0.7301 0.238 Uiso 1 1 calc R . .
H25C H 1.3139 0.7938 0.6496 0.238 Uiso 1 1 calc R . .
C26 C 1.4030(7) 0.8518(6) 0.8086(10) 0.234(6) Uani 1 1 d . . .
H26A H 1.4071 0.8859 0.8545 0.351 Uiso 1 1 calc R . .
H26B H 1.4310 0.8670 0.7565 0.351 Uiso 1 1 calc R . .
H26C H 1.4413 0.8145 0.8365 0.351 Uiso 1 1 calc R . .
C27 C 0.9662(6) 0.9653(3) 0.7612(6) 0.112(2) Uani 1 1 d . . .
H27A H 0.9608 0.9344 0.8116 0.135 Uiso 1 1 calc R . .
C28 C 0.8724(7) 0.9572(5) 0.6839(8) 0.166(4) Uani 1 1 d . . .
H28A H 0.8121 0.9671 0.7081 0.249 Uiso 1 1 calc R . .
H28B H 0.8687 0.9130 0.6614 0.249 Uiso 1 1 calc R . .
H28C H 0.8766 0.9864 0.6331 0.249 Uiso 1 1 calc R . .
C29 C 0.9660(10) 1.0336(5) 0.8003(8) 0.216(6) Uani 1 1 d . . .
H29A H 0.9025 1.0412 0.8202 0.324 Uiso 1 1 calc R . .
H29B H 0.9734 1.0646 0.7525 0.324 Uiso 1 1 calc R . .
H29C H 1.0220 1.0383 0.8532 0.324 Uiso 1 1 calc R . .
C36 C 0.9104(5) 0.7767(2) 0.5838(4) 0.0728(15) Uani 1 1 d D . .
C37 C 0.8207(5) 0.7700(3) 0.5179(5) 0.0903(19) Uani 1 1 d . . .
H37A H 0.7691 0.7433 0.5317 0.108 Uiso 1 1 calc R . .
C41 C 0.9846(5) 0.8166(3) 0.5578(5) 0.0905(18) Uani 1 1 d D . .
H41A H 1.0461 0.8230 0.6005 0.109 Uiso 1 1 calc R . .
C40 C 0.9707(6) 0.8467(3) 0.4722(5) 0.0945(19) Uani 1 1 d . . .
H40A H 1.0228 0.8718 0.4562 0.113 Uiso 1 1 calc R . .
C30 C 0.9473(7) 0.6545(3) 0.6743(5) 0.104(2) Uani 1 1 d D . .
C38 C 0.8053(6) 0.8009(3) 0.4340(5) 0.101(2) Uani 1 1 d . . .
H38A H 0.7432 0.7960 0.3916 0.122 Uiso 1 1 calc R . .
C39 C 0.8804(7) 0.8394(3) 0.4113(5) 0.099(2) Uani 1 1 d . . .
H39A H 0.8693 0.8606 0.3534 0.119 Uiso 1 1 calc R . .
C35 C 1.0169(9) 0.6298(5) 0.6319(8) 0.168(4) Uani 1 1 d D . .
H35A H 1.0597 0.6592 0.6095 0.202 Uiso 1 1 calc R . .
C31 C 0.8810(7) 0.6085(4) 0.7013(6) 0.133(3) Uani 1 1 d . . .
H31A H 0.8275 0.6226 0.7289 0.160 Uiso 1 1 calc R . .
C33 C 0.9712(15) 0.5253(7) 0.6457(11) 0.198(9) Uani 1 1 d . . .
H33A H 0.9814 0.4810 0.6363 0.238 Uiso 1 1 calc R . .
C34 C 1.0320(16) 0.5660(7) 0.6178(11) 0.242(9) Uani 1 1 d . . .
H34A H 1.0846 0.5519 0.5890 0.290 Uiso 1 1 calc R . .
C32 C 0.8938(12) 0.5423(6) 0.6875(10) 0.185(6) Uani 1 1 d . . .
H32A H 0.8510 0.5113 0.7063 0.222 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'
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'
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 N1 97.35(17) . . ?
N2 Ni1 P1A 124.1(4) . . ?
N1 Ni1 P1A 133.1(3) . . ?
N2 Ni1 P1 148.45(14) . . ?
N1 Ni1 P1 112.74(13) . . ?
P1A Ni1 P1 36.2(4) . . ?
P1A P1 C30 76.6(5) . . ?
P1A P1 C36 81.5(5) . . ?
C30 P1 C36 102.4(3) . . ?
P1A P1 Ni1 65.7(4) . . ?
C30 P1 Ni1 121.7(3) . . ?
C36 P1 Ni1 113.3(2) . . ?
P1 P1A C30 63.0(5) . . ?
P1 P1A Ni1 78.0(6) . . ?
C30 P1A Ni1 121.1(7) . . ?
P1 P1A C36 59.6(5) . . ?
C30 P1A C36 88.3(5) . . ?
Ni1 P1A C36 108.8(6) . . ?
C14 N1 C1 120.0(4) . . ?
C14 N1 Ni1 123.3(3) . . ?
C1 N1 Ni1 116.5(3) . . ?
C16 N2 C18 120.6(4) . . ?
C16 N2 Ni1 124.5(3) . . ?
C18 N2 Ni1 114.6(3) . . ?
C2 C1 C6 121.4(5) . . ?
C2 C1 N1 120.5(4) . . ?
C6 C1 N1 117.9(4) . . ?
C1 C2 C3 117.7(5) . . ?
C1 C2 C7 122.1(5) . . ?
C3 C2 C7 120.2(5) . . ?
C4 C3 C2 121.1(6) . . ?
C3 C4 C5 120.5(6) . . ?
C4 C5 C6 121.7(6) . . ?
C5 C6 C1 117.6(5) . . ?
C5 C6 C10 120.5(5) . . ?
C1 C6 C10 121.9(5) . . ?
C2 C7 C8 112.0(5) . . ?
C2 C7 C9 112.2(6) . . ?
C8 C7 C9 109.4(6) . . ?
C12 C10 C6 113.0(6) . . ?
C12 C10 C11 106.8(7) . . ?
C6 C10 C11 114.3(6) . . ?
N1 C14 C15 122.6(5) . . ?
N1 C14 C13 120.6(5) . . ?
C15 C14 C13 116.9(5) . . ?
C14 C15 C16 129.2(5) . . ?
N2 C16 C15 122.7(5) . . ?
N2 C16 C17 120.2(5) . . ?
C15 C16 C17 117.0(5) . . ?
C23 C18 C19 121.3(5) . . ?
C23 C18 N2 119.5(5) . . ?
C19 C18 N2 119.2(5) . . ?
C20 C19 C18 117.3(6) . . ?
C20 C19 C24 120.6(6) . . ?
C18 C19 C24 122.0(5) . . ?
C21 C20 C19 122.1(7) . . ?
C20 C21 C22 120.4(7) . . ?
C23 C22 C21 120.3(7) . . ?
C22 C23 C18 118.5(6) . . ?
C22 C23 C27 119.5(6) . . ?
C18 C23 C27 122.0(5) . . ?
C19 C24 C26 114.9(7) . . ?
C19 C24 C25 110.2(6) . . ?
C26 C24 C25 109.0(8) . . ?
C28 C27 C29 108.4(8) . . ?
C28 C27 C23 112.3(7) . . ?
C29 C27 C23 111.9(7) . . ?
C37 C36 C41 115.7(5) . . ?
C37 C36 P1 120.1(5) . . ?
C41 C36 P1 124.1(5) . . ?
C37 C36 P1A 150.6(5) . . ?
C41 C36 P1A 89.7(5) . . ?
P1 C36 P1A 38.9(4) . . ?
C38 C37 C36 122.1(6) . . ?
C40 C41 C36 122.6(6) . . ?
C39 C40 C41 119.0(6) . . ?
C35 C30 C31 114.6(7) . . ?
C35 C30 P1 129.1(7) . . ?
C31 C30 P1 116.3(7) . . ?
C35 C30 P1A 91.4(7) . . ?
C31 C30 P1A 150.8(7) . . ?
P1 C30 P1A 40.5(4) . . ?
C37 C38 C39 120.2(7) . . ?
C40 C39 C38 120.3(7) . . ?
C30 C35 C34 125.9(11) . . ?
C32 C31 C30 121.0(11) . . ?
C34 C33 C32 124.3(16) . . ?
C33 C34 C35 117.4(16) . . ?
C33 C32 C31 116.6(13) . . ?
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 1.884(4) . ?
Ni1 N1 1.919(4) . ?
Ni1 P1A 2.034(11) . ?
Ni1 P1 2.1824(18) . ?
P1 P1A 1.319(14) . ?
P1 C30 1.809(7) . ?
P1 C36 1.810(6) . ?
P1A C30 1.976(11) . ?
P1A C36 2.075(12) . ?
N1 C14 1.335(6) . ?
N1 C1 1.437(6) . ?
N2 C16 1.317(6) . ?
N2 C18 1.429(6) . ?
C1 C2 1.397(7) . ?
C1 C6 1.404(7) . ?
C2 C3 1.399(7) . ?
C2 C7 1.520(8) . ?
C3 C4 1.359(9) . ?
C4 C5 1.364(8) . ?
C5 C6 1.381(8) . ?
C6 C10 1.499(8) . ?
C7 C8 1.521(9) . ?
C7 C9 1.530(9) . ?
C10 C12 1.492(10) . ?
C10 C11 1.513(9) . ?
C13 C14 1.506(7) . ?
C14 C15 1.386(7) . ?
C15 C16 1.402(7) . ?
C16 C17 1.513(7) . ?
C18 C23 1.393(8) . ?
C18 C19 1.408(7) . ?
C19 C20 1.389(8) . ?
C19 C24 1.489(8) . ?
C20 C21 1.342(10) . ?
C21 C22 1.389(10) . ?
C22 C23 1.386(8) . ?
C23 C27 1.529(9) . ?
C24 C26 1.513(10) . ?
C24 C25 1.516(9) . ?
C27 C28 1.508(11) . ?
C27 C29 1.509(11) . ?
C36 C37 1.377(8) . ?
C36 C41 1.390(8) . ?
C37 C38 1.350(9) . ?
C41 C40 1.365(8) . ?
C40 C39 1.349(9) . ?
C30 C35 1.314(11) . ?
C30 C31 1.399(11) . ?
C38 C39 1.365(9) . ?
C35 C34 1.344(13) . ?
C31 C32 1.385(14) . ?
C33 C34 1.284(19) . ?
C33 C32 1.344(18) . ?
