#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/67/7006780.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_7006780
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            'C38.5 H50 Fe N2 P'
_chemical_formula_weight         627.63
_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                 92.8560(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1127(6)
_cell_length_b                   14.2879(7)
_cell_length_c                   19.5668(9)
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     3661.3(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(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  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0498
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17870
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.477
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.737894
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_density_diffrn    1.055
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.178
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.905
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5262
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.905
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0866P)²+1.8524P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1446
_reflns_number_gt                3522
_reflns_number_total             5262
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b513892b.txt
_cod_data_source_block           '[(NacNac)Fe(??-PPh)]2.Toluene'
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C38.50 H50 Fe N2 P'
_cod_database_code               7006780
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
Fe1 Fe 0.10644(4) 0.40743(3) 0.01114(3) 0.0450(2) Uani 1 1 d . . .
P1 P 0.07854(8) 0.57713(7) 0.01374(5) 0.0524(3) Uani 1 1 d . . .
N1 N 0.1503(2) 0.3392(2) 0.09780(14) 0.0458(7) Uani 1 1 d . . .
N2 N 0.2262(2) 0.3648(2) -0.04118(15) 0.0501(8) Uani 1 1 d . . .
C1 C 0.0788(3) 0.3243(3) 0.15079(19) 0.0511(9) Uani 1 1 d . . .
C2 C 0.0222(3) 0.2406(3) 0.1495(2) 0.0635(11) Uani 1 1 d . . .
C3 C -0.0427(4) 0.2250(4) 0.2020(3) 0.0869(16) Uani 1 1 d . . .
H3A H -0.0784 0.1688 0.2033 0.104 Uiso 1 1 calc R . .
C4 C -0.0554(4) 0.2906(5) 0.2521(3) 0.0914(17) Uani 1 1 d . . .
H4A H -0.0993 0.2787 0.2869 0.110 Uiso 1 1 calc R . .
C5 C -0.0034(4) 0.3736(4) 0.2507(2) 0.0775(14) Uani 1 1 d . . .
H5A H -0.0140 0.4181 0.2843 0.093 Uiso 1 1 calc R . .
C6 C 0.0649(3) 0.3930(3) 0.20024(19) 0.0580(10) Uani 1 1 d . . .
C7 C 0.0300(4) 0.1690(3) 0.0923(3) 0.0775(13) Uani 1 1 d . . .
H7A H 0.0472 0.2038 0.0513 0.093 Uiso 1 1 calc R . .
C8 C -0.0701(5) 0.1179(4) 0.0747(3) 0.118(2) Uani 1 1 d . . .
H8A H -0.1235 0.1627 0.0654 0.177 Uiso 1 1 calc R . .
H8B H -0.0874 0.0793 0.1127 0.177 Uiso 1 1 calc R . .
H8C H -0.0625 0.0793 0.0351 0.177 Uiso 1 1 calc R . .
C9 C 0.1147(5) 0.0979(4) 0.1062(4) 0.130(2) Uani 1 1 d . . .
H9A H 0.1773 0.1299 0.1186 0.195 Uiso 1 1 calc R . .
H9B H 0.1235 0.0613 0.0657 0.195 Uiso 1 1 calc R . .
H9C H 0.0970 0.0574 0.1429 0.195 Uiso 1 1 calc R . .
C10 C 0.1208(3) 0.4849(3) 0.2005(2) 0.0656(12) Uani 1 1 d . . .
H10A H 0.1581 0.4877 0.1583 0.079 Uiso 1 1 calc R . .
C11 C 0.0493(5) 0.5678(4) 0.2000(3) 0.1037(18) Uani 1 1 d . . .
H11A H 0.0003 0.5624 0.1620 0.156 Uiso 1 1 calc R . .
H11B H 0.0878 0.6245 0.1956 0.156 Uiso 1 1 calc R . .
H11C H 0.0144 0.5692 0.2419 0.156 Uiso 1 1 calc R . .
C12 C 0.1990(5) 0.4939(4) 0.2602(3) 0.110(2) Uani 1 1 d . . .
H12A H 0.2449 0.4415 0.2602 0.164 Uiso 1 1 calc R . .
H12B H 0.1646 0.4949 0.3024 0.164 Uiso 1 1 calc R . .
H12C H 0.2369 0.5509 0.2557 0.164 Uiso 1 1 calc R . .
C13 C 0.2828(3) 0.2753(3) 0.1800(2) 0.0731(13) Uani 1 1 d . . .
H13A H 0.3174 0.3242 0.2055 0.110 Uiso 1 1 calc R . .
H13B H 0.3288 0.2238 0.1744 0.110 Uiso 1 1 calc R . .
H13C H 0.2251 0.2544 0.2041 0.110 Uiso 1 1 calc R . .
C14 C 0.2467(3) 0.3121(3) 0.11014(19) 0.0522(10) Uani 1 1 d . . .
C15 C 0.3195(3) 0.3134(3) 0.0606(2) 0.0617(11) Uani 1 1 d . . .
H15A H 0.3856 0.2999 0.0772 0.074 Uiso 1 1 calc R . .
C16 C 0.3103(3) 0.3313(3) -0.0093(2) 0.0566(10) Uani 1 1 d . . .
C17 C 0.4034(3) 0.3055(4) -0.0484(2) 0.0816(14) Uani 1 1 d . . .
H17A H 0.4154 0.2394 -0.0446 0.122 Uiso 1 1 calc R . .
H17B H 0.4618 0.3389 -0.0296 0.122 Uiso 1 1 calc R . .
H17C H 0.3917 0.3219 -0.0957 0.122 Uiso 1 1 calc R . .
C18 C 0.2241(3) 0.3736(3) -0.1149(2) 0.0557(10) Uani 1 1 d . . .
C19 C 0.2634(3) 0.4526(3) -0.1455(2) 0.0664(12) Uani 1 1 d . . .
C20 C 0.2595(4) 0.4573(5) -0.2161(3) 0.0910(16) Uani 1 1 d . . .
H20A H 0.2860 0.5096 -0.2373 0.109 Uiso 1 1 calc R . .
C21 C 0.2184(5) 0.3882(6) -0.2550(3) 0.103(2) Uani 1 1 d . . .
H21A H 0.2175 0.3932 -0.3024 0.123 Uiso 1 1 calc R . .
C22 C 0.1777(4) 0.3104(5) -0.2257(3) 0.0919(17) Uani 1 1 d . . .
H22A H 0.1494 0.2632 -0.2534 0.110 Uiso 1 1 calc R . .
C23 C 0.1783(3) 0.3014(3) -0.1546(2) 0.0675(12) Uani 1 1 d . . .
C24 C 0.3103(4) 0.5326(4) -0.1053(3) 0.0902(16) Uani 1 1 d . . .
H24A H 0.2960 0.5234 -0.0571 0.108 Uiso 1 1 calc R . .
C25 C 0.2662(5) 0.6278(4) -0.1280(3) 0.123(2) Uani 1 1 d . . .
H25A H 0.1935 0.6274 -0.1241 0.185 Uiso 1 1 calc R . .
H25B H 0.2815 0.6393 -0.1747 0.185 Uiso 1 1 calc R . .
H25C H 0.2959 0.6762 -0.0994 0.185 Uiso 1 1 calc R . .
C26 C 0.4279(5) 0.5375(6) -0.1107(4) 0.163(3) Uani 1 1 d . . .
H26A H 0.4579 0.4796 -0.0951 0.245 Uiso 1 1 calc R . .
H26B H 0.4548 0.5879 -0.0828 0.245 Uiso 1 1 calc R . .
H26C H 0.4436 0.5480 -0.1575 0.245 Uiso 1 1 calc R . .
C27 C 0.1320(4) 0.2156(3) -0.1221(3) 0.0862(15) Uani 1 1 d . . .
H27A H 0.1024 0.2366 -0.0798 0.103 Uiso 1 1 calc R . .
C28 C 0.2110(5) 0.1411(4) -0.1022(4) 0.135(2) Uani 1 1 d . . .
H28A H 0.2654 0.1687 -0.0744 0.202 Uiso 1 1 calc R . .
H28B H 0.2380 0.1150 -0.1427 0.202 Uiso 1 1 calc R . .
H28C H 0.1794 0.0924 -0.0768 0.202 Uiso 1 1 calc R . .
C29 C 0.0454(4) 0.1707(4) -0.1662(3) 0.117(2) Uani 1 1 d . . .
H29A H 0.0188 0.1180 -0.1425 0.176 Uiso 1 1 calc R . .
H29B H 0.0711 0.1504 -0.2089 0.176 Uiso 1 1 calc R . .
H29C H -0.0080 0.2158 -0.1750 0.176 Uiso 1 1 calc R . .
C30 C 0.1753(3) 0.6523(3) 0.0568(2) 0.0566(10) Uani 1 1 d . . .
C31 C 0.1559(4) 0.7452(3) 0.0680(3) 0.0849(15) Uani 1 1 d . . .
H31A H 0.0942 0.7708 0.0516 0.102 Uiso 1 1 calc R . .
C32 C 0.2261(5) 0.8013(4) 0.1030(4) 0.122(2) Uani 1 1 d . . .
H32A H 0.2119 0.8642 0.1101 0.146 Uiso 1 1 calc R . .
C33 C 0.3160(5) 0.7642(5) 0.1271(3) 0.119(2) Uani 1 1 d . . .
H33A H 0.3634 0.8019 0.1509 0.143 Uiso 1 1 calc R . .
C34 C 0.3373(4) 0.6723(4) 0.1168(3) 0.0923(16) Uani 1 1 d . . .
H34A H 0.3992 0.6475 0.1335 0.111 Uiso 1 1 calc R . .
C35 C 0.2673(3) 0.6158(3) 0.0817(2) 0.0697(12) Uani 1 1 d . . .
H35A H 0.2821 0.5529 0.0747 0.084 Uiso 1 1 calc R . .
C36 C 0.4043(14) -0.0989(12) -0.0479(9) 0.283(7) Uiso 1 1 d . . .
C37 C 0.3865(17) -0.0220(16) 0.0055(12) 0.167(7) Uiso 0.50 1 d P . .
C38 C 0.4364(13) 0.0312(10) 0.0379(7) 0.212(4) Uiso 1 1 d . . .
C39 C 0.540(2) 0.0373(17) 0.0174(13) 0.188(8) Uiso 0.50 1 d P . .
C40 C 0.5042(17) 0.0917(13) 0.0785(10) 0.165(6) Uiso 0.50 1 d P . .
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'
Fe Fe 0.3463 0.8444 '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 Fe1 N1 94.83(12) . . ?
N2 Fe1 P1 115.54(9) . . ?
N1 Fe1 P1 119.84(9) . . ?
N2 Fe1 P1 135.53(9) . 3_565 ?
N1 Fe1 P1 116.57(9) . 3_565 ?
P1 Fe1 P1 76.64(4) . 3_565 ?
C30 P1 Fe1 119.19(14) . . ?
C30 P1 Fe1 133.69(14) . 3_565 ?
Fe1 P1 Fe1 103.36(4) . 3_565 ?
C14 N1 C1 118.0(3) . . ?
C14 N1 Fe1 121.4(2) . . ?
C1 N1 Fe1 120.4(2) . . ?
C16 N2 C18 118.3(3) . . ?
C16 N2 Fe1 121.4(3) . . ?
C18 N2 Fe1 120.3(2) . . ?
C6 C1 C2 121.5(4) . . ?
C6 C1 N1 120.3(3) . . ?
C2 C1 N1 118.2(3) . . ?
C3 C2 C1 117.9(4) . . ?
C3 C2 C7 120.2(4) . . ?
C1 C2 C7 121.9(4) . . ?
C4 C3 C2 121.3(5) . . ?
C5 C4 C3 120.0(4) . . ?
C4 C5 C6 121.6(5) . . ?
C5 C6 C1 117.5(4) . . ?
C5 C6 C10 120.2(4) . . ?
C1 C6 C10 122.4(3) . . ?
C9 C7 C2 113.2(4) . . ?
C9 C7 C8 109.4(4) . . ?
C2 C7 C8 113.5(5) . . ?
C6 C10 C11 112.5(4) . . ?
C6 C10 C12 112.7(4) . . ?
C11 C10 C12 109.5(4) . . ?
N1 C14 C15 123.1(3) . . ?
N1 C14 C13 120.9(3) . . ?
C15 C14 C13 115.9(3) . . ?
C16 C15 C14 131.1(4) . . ?
N2 C16 C15 123.8(4) . . ?
N2 C16 C17 121.4(4) . . ?
C15 C16 C17 114.8(4) . . ?
C19 C18 C23 121.0(4) . . ?
C19 C18 N2 120.8(4) . . ?
C23 C18 N2 118.2(4) . . ?
C20 C19 C18 118.3(5) . . ?
C20 C19 C24 118.7(5) . . ?
C18 C19 C24 123.0(4) . . ?
C21 C20 C19 121.7(5) . . ?
C20 C21 C22 120.8(5) . . ?
C21 C22 C23 120.6(5) . . ?
C22 C23 C18 117.6(5) . . ?
C22 C23 C27 120.5(5) . . ?
C18 C23 C27 121.9(4) . . ?
C19 C24 C25 112.6(5) . . ?
C19 C24 C26 112.4(5) . . ?
C25 C24 C26 107.6(5) . . ?
C23 C27 C28 113.0(5) . . ?
C23 C27 C29 113.7(5) . . ?
C28 C27 C29 109.1(4) . . ?
C31 C30 C35 118.5(4) . . ?
C31 C30 P1 120.6(3) . . ?
C35 C30 P1 120.8(3) . . ?
C30 C31 C32 121.2(5) . . ?
C33 C32 C31 119.6(6) . . ?
C32 C33 C34 120.5(5) . . ?
C33 C34 C35 120.1(5) . . ?
C30 C35 C34 120.1(5) . . ?
C39 C36 C40 69.8(18) 3_655 3_655 ?
C39 C36 C37 45.2(14) 3_655 . ?
C40 C36 C37 114.1(17) 3_655 . ?
C39 C37 C38 83(2) 3_655 . ?
C39 C37 C36 54.6(17) 3_655 . ?
C38 C37 C36 137(2) . . ?
C37 C38 C39 114(2) . . ?
C37 C38 C40 176(2) . . ?
C39 C38 C40 63.5(14) . . ?
C37 C38 C39 47.1(13) . 3_655 ?
C39 C38 C39 66.6(19) . 3_655 ?
C40 C38 C39 130(2) . 3_655 ?
C37 C39 C36 80(2) 3_655 3_655 ?
C37 C39 C38 163(3) 3_655 . ?
C36 C39 C38 116(3) 3_655 . ?
C37 C39 C38 50.3(17) 3_655 3_655 ?
C36 C39 C38 130(3) 3_655 3_655 ?
C38 C39 C38 113.4(19) . 3_655 ?
C37 C39 C40 137(3) 3_655 . ?
C36 C39 C40 58.0(15) 3_655 . ?
C38 C39 C40 58.8(16) . . ?
C38 C39 C40 170(2) 3_655 . ?
C37 C39 C39 105(3) 3_655 3_655 ?
C36 C39 C39 175(4) 3_655 3_655 ?
C38 C39 C39 58.8(18) . 3_655 ?
C38 C39 C39 54.6(15) 3_655 3_655 ?
C40 C39 C39 117(3) . 3_655 ?
C36 C40 C38 109.4(16) 3_655 . ?
C36 C40 C39 52.2(13) 3_655 . ?
C38 C40 C39 57.7(11) . . ?
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
Fe1 N2 2.012(3) . ?
Fe1 N1 2.015(3) . ?
Fe1 P1 2.4530(11) . ?
Fe1 P1 2.4599(11) 3_565 ?
P1 C30 1.836(4) . ?
P1 Fe1 2.4599(11) 3_565 ?
N1 C14 1.333(5) . ?
N1 C1 1.448(4) . ?
N2 C16 1.329(5) . ?
N2 C18 1.447(5) . ?
C1 C6 1.397(5) . ?
C1 C2 1.406(5) . ?
C2 C3 1.384(6) . ?
C2 C7 1.523(6) . ?
C3 C4 1.372(7) . ?
C4 C5 1.368(7) . ?
C5 C6 1.394(6) . ?
C6 C10 1.503(6) . ?
C7 C9 1.520(7) . ?
C7 C8 1.527(7) . ?
C10 C11 1.510(6) . ?
C10 C12 1.522(6) . ?
C13 C14 1.517(5) . ?
C14 C15 1.393(5) . ?
C15 C16 1.392(5) . ?
C16 C17 1.517(5) . ?
C18 C19 1.388(6) . ?
C18 C23 1.408(6) . ?
C19 C20 1.382(6) . ?
C19 C24 1.501(7) . ?
C20 C21 1.343(8) . ?
C21 C22 1.371(8) . ?
C22 C23 1.397(6) . ?
C23 C27 1.520(6) . ?
C24 C25 1.535(7) . ?
C24 C26 1.552(8) . ?
C27 C28 1.523(7) . ?
C27 C29 1.533(7) . ?
C30 C31 1.371(6) . ?
C30 C35 1.380(6) . ?
C31 C32 1.376(7) . ?
C32 C33 1.355(8) . ?
C33 C34 1.359(8) . ?
C34 C35 1.381(6) . ?
C36 C39 1.28(2) 3_655 ?
C36 C40 1.37(2) 3_655 ?
C36 C37 1.54(3) . ?
C37 C39 1.11(3) 3_655 ?
C37 C38 1.17(2) . ?
C38 C39 1.43(2) . ?
C38 C40 1.45(2) . ?
C38 C39 1.50(3) 3_655 ?
C39 C37 1.11(3) 3_655 ?
C39 C36 1.28(2) 3_655 ?
C39 C38 1.50(3) 3_655 ?
C39 C40 1.52(3) . ?
C39 C39 1.61(5) 3_655 ?
C40 C36 1.37(2) 3_655 ?
