#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:29:25 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179450 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/47/4334748.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_4334748
loop_
_publ_author_name
'Kanghee Park'
'Paraskevi O. Lagaditis'
'Alan J. Lough'
'Robert H. Morris'
_publ_section_title
;
 Synthesis of New Late Transition Metal P,P-, P,N-, and P,O- Complexes
 Using Phosphonium Dimers as Convenient Ligand Precursors
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5448
_journal_page_last               5456
_journal_paper_doi               10.1021/ic4003753
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C28 H48 Ni O2 P2'
_chemical_formula_sum            'C28 H48 Ni O2 P2'
_chemical_formula_weight         537.31
_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                97.088(3)
_cell_angle_beta                 109.224(3)
_cell_angle_gamma                114.046(3)
_cell_formula_units_Z            2
_cell_length_a                   9.8176(7)
_cell_length_b                   11.9293(7)
_cell_length_c                   14.3536(10)
_cell_measurement_reflns_used    18331
_cell_measurement_temperature    147(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.9
_cell_volume                     1383.39(17)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius B.V., 1997-2002)'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      147(1)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offsets'
_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  0.0730
_diffrn_reflns_av_sigmaI/netI    0.0746
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18331
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.86
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.840
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       needle
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.179
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         6286
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0562
_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)+(0.0742P)²+0.3363P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1463
_reflns_number_gt                4337
_reflns_number_total             6286
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic4003753_si_001_1.cif
_cod_data_source_block           2a
_cod_original_cell_volume        1383.39(16)
_cod_database_code               4334748
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
Ni1A Ni 1.0000 0.5000 0.5000 0.02972(16) Uani 1 2 d S
P1A P 0.76070(10) 0.32110(7) 0.43236(6) 0.0298(2) Uani 1 1 d .
O1A O 0.8862(3) 0.58722(19) 0.51844(17) 0.0358(5) Uani 1 1 d .
C1A C 0.6369(4) 0.3908(3) 0.4459(3) 0.0327(7) Uani 1 1 d .
H1A H 0.5217 0.3434 0.4249 0.039 Uiso 1 1 calc R
C2A C 0.7260(4) 0.5187(3) 0.4895(2) 0.0338(7) Uani 1 1 d .
H2A H 0.6695 0.5638 0.5005 0.041 Uiso 1 1 calc R
C3A C 0.6826(4) 0.2361(3) 0.2947(2) 0.0300(7) Uani 1 1 d .
H3AA H 0.7494 0.1931 0.2889 0.036 Uiso 1 1 calc R
C4A C 0.5024(4) 0.1322(3) 0.2480(3) 0.0370(7) Uani 1 1 d .
H4AA H 0.4352 0.1711 0.2595 0.044 Uiso 1 1 calc R
H4AB H 0.4910 0.0653 0.2838 0.044 Uiso 1 1 calc R
C5A C 0.4370(4) 0.0692(3) 0.1316(3) 0.0404(8) Uani 1 1 d .
H5AA H 0.4948 0.0210 0.1204 0.048 Uiso 1 1 calc R
H5AB H 0.3185 0.0072 0.1039 0.048 Uiso 1 1 calc R
C6A C 0.4617(4) 0.1688(3) 0.0737(3) 0.0380(8) Uani 1 1 d .
H6AA H 0.3942 0.2105 0.0783 0.046 Uiso 1 1 calc R
H6AB H 0.4249 0.1260 -0.0002 0.046 Uiso 1 1 calc R
C7A C 0.6420(4) 0.2703(3) 0.1189(3) 0.0409(8) Uani 1 1 d .
H7AA H 0.6541 0.3367 0.0825 0.049 Uiso 1 1 calc R
H7AB H 0.7072 0.2296 0.1071 0.049 Uiso 1 1 calc R
C8A C 0.7093(4) 0.3345(3) 0.2345(3) 0.0365(7) Uani 1 1 d .
H8AA H 0.6544 0.3852 0.2456 0.044 Uiso 1 1 calc R
H8AB H 0.8283 0.3946 0.2614 0.044 Uiso 1 1 calc R
C9A C 0.7298(4) 0.1969(3) 0.4994(2) 0.0315(7) Uani 1 1 d .
H9AA H 0.6098 0.1342 0.4676 0.038 Uiso 1 1 calc R
C10A C 0.7789(4) 0.2578(3) 0.6136(3) 0.0386(8) Uani 1 1 d .
H10A H 0.8972 0.3215 0.6470 0.046 Uiso 1 1 calc R
H10B H 0.7161 0.3036 0.6190 0.046 Uiso 1 1 calc R
C11A C 0.7452(4) 0.1557(3) 0.6695(3) 0.0394(8) Uani 1 1 d .
H11A H 0.6254 0.0976 0.6408 0.047 Uiso 1 1 calc R
H11B H 0.7837 0.1979 0.7437 0.047 Uiso 1 1 calc R
C12A C 0.8318(4) 0.0771(3) 0.6581(3) 0.0420(8) Uani 1 1 d .
H12A H 0.9520 0.1331 0.6957 0.050 Uiso 1 1 calc R
H12B H 0.7993 0.0071 0.6898 0.050 Uiso 1 1 calc R
C13A C 0.7899(4) 0.0194(3) 0.5454(3) 0.0408(8) Uani 1 1 d .
H13A H 0.6729 -0.0470 0.5103 0.049 Uiso 1 1 calc R
H13B H 0.8571 -0.0230 0.5420 0.049 Uiso 1 1 calc R
C14A C 0.8211(4) 0.1218(3) 0.4884(3) 0.0350(7) Uani 1 1 d .
H14A H 0.9404 0.1819 0.5172 0.042 Uiso 1 1 calc R
H14B H 0.7837 0.0796 0.4142 0.042 Uiso 1 1 calc R
Ni1B Ni 0.0000 0.5000 0.0000 0.02958(16) Uani 1 2 d S
P1B P 0.19778(10) 0.45695(7) 0.08422(6) 0.0295(2) Uani 1 1 d .
O1B O 0.0231(3) 0.4491(2) -0.11967(16) 0.0358(5) Uani 1 1 d .
C1B C 0.2439(4) 0.4172(3) -0.0208(2) 0.0331(7) Uani 1 1 d .
H1B H 0.3308 0.3981 -0.0151 0.040 Uiso 1 1 calc R
C2B C 0.1400(4) 0.4176(3) -0.1098(3) 0.0364(7) Uani 1 1 d .
H2B H 0.1522 0.3930 -0.1709 0.044 Uiso 1 1 calc R
C3B C 0.3791(4) 0.5960(3) 0.1883(2) 0.0299(7) Uani 1 1 d .
H3BA H 0.3468 0.6152 0.2450 0.036 Uiso 1 1 calc R
C4B C 0.4291(4) 0.7147(3) 0.1499(3) 0.0358(7) Uani 1 1 d .
H4BA H 0.4560 0.6969 0.0909 0.043 Uiso 1 1 calc R
H4BB H 0.3356 0.7327 0.1251 0.043 Uiso 1 1 calc R
C5B C 0.5770(4) 0.8323(3) 0.2353(3) 0.0394(8) Uani 1 1 d .
H5BA H 0.5468 0.8551 0.2914 0.047 Uiso 1 1 calc R
H5BB H 0.6092 0.9061 0.2073 0.047 Uiso 1 1 calc R
C6B C 0.7222(4) 0.8068(3) 0.2790(3) 0.0385(8) Uani 1 1 d .
H6BA H 0.7591 0.7918 0.2245 0.046 Uiso 1 1 calc R
H6BB H 0.8147 0.8831 0.3364 0.046 Uiso 1 1 calc R
C7B C 0.6740(4) 0.6898(3) 0.3184(3) 0.0406(8) Uani 1 1 d .
H7BA H 0.7679 0.6722 0.3429 0.049 Uiso 1 1 calc R
H7BB H 0.6485 0.7087 0.3778 0.049 Uiso 1 1 calc R
C8B C 0.5261(4) 0.5717(3) 0.2348(3) 0.0365(7) Uani 1 1 d .
H8BA H 0.4940 0.4995 0.2645 0.044 Uiso 1 1 calc R
H8BB H 0.5561 0.5466 0.1793 0.044 Uiso 1 1 calc R
C9B C 0.1582(4) 0.3218(3) 0.1397(2) 0.0313(7) Uani 1 1 d .
H9BA H 0.2584 0.3104 0.1600 0.038 Uiso 1 1 calc R
C10B C 0.1297(4) 0.3464(3) 0.2376(3) 0.0363(7) Uani 1 1 d .
H10C H 0.2274 0.4241 0.2908 0.044 Uiso 1 1 calc R
H10D H 0.0344 0.3626 0.2210 0.044 Uiso 1 1 calc R
C11B C 0.0976(4) 0.2313(3) 0.2807(3) 0.0381(8) Uani 1 1 d .
H11C H 0.1990 0.2234 0.3067 0.046 Uiso 1 1 calc R
H11D H 0.0697 0.2467 0.3396 0.046 Uiso 1 1 calc R
C12B C -0.0415(4) 0.1061(3) 0.1994(3) 0.0377(8) Uani 1 1 d .
H12C H -0.1462 0.1089 0.1807 0.045 Uiso 1 1 calc R
H12D H -0.0511 0.0336 0.2285 0.045 Uiso 1 1 calc R
C13B C -0.0121(4) 0.0834(3) 0.1025(3) 0.0361(7) Uani 1 1 d .
H13C H -0.1081 0.0046 0.0496 0.043 Uiso 1 1 calc R
H13D H 0.0852 0.0698 0.1195 0.043 Uiso 1 1 calc R
C14B C 0.0156(4) 0.1970(3) 0.0586(3) 0.0347(7) Uani 1 1 d .
H14C H 0.0394 0.1810 -0.0021 0.042 Uiso 1 1 calc R
H14D H -0.0856 0.2055 0.0353 0.042 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'
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'
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
O1A Ni1A O1A 180.00(15) 2_766 .
O1A Ni1A P1A 87.04(7) 2_766 2_766
O1A Ni1A P1A 92.96(7) . 2_766
O1A Ni1A P1A 92.96(7) 2_766 .
O1A Ni1A P1A 87.04(7) . .
P1A Ni1A P1A 180.00(7) 2_766 .
C1A P1A C9A 107.20(14) . .
C1A P1A C3A 108.79(15) . .
C9A P1A C3A 106.25(14) . .
C1A P1A Ni1A 97.96(11) . .
C9A P1A Ni1A 119.03(11) . .
C3A P1A Ni1A 116.63(10) . .
C2A O1A Ni1A 117.93(19) . .
C2A C1A P1A 111.7(2) . .
O1A C2A C1A 125.4(3) . .
C8A C3A C4A 111.1(3) . .
C8A C3A P1A 109.0(2) . .
C4A C3A P1A 113.3(2) . .
C3A C4A C5A 112.2(3) . .
C6A C5A C4A 111.4(3) . .
C5A C6A C7A 110.6(3) . .
C6A C7A C8A 112.2(3) . .
C7A C8A C3A 111.9(3) . .
C14A C9A C10A 110.8(3) . .
C14A C9A P1A 113.2(2) . .
C10A C9A P1A 109.9(2) . .
C11A C10A C9A 110.9(3) . .
C10A C11A C12A 111.4(3) . .
C13A C12A C11A 112.0(3) . .
C12A C13A C14A 111.9(3) . .
C9A C14A C13A 110.7(2) . .
O1B Ni1B O1B 180.00(12) . 2_565
O1B Ni1B P1B 87.32(7) . .
O1B Ni1B P1B 92.68(7) 2_565 .
O1B Ni1B P1B 92.68(7) . 2_565
O1B Ni1B P1B 87.32(7) 2_565 2_565
P1B Ni1B P1B 180.0 . 2_565
C1B P1B C3B 110.40(15) . .
C1B P1B C9B 106.94(14) . .
C3B P1B C9B 105.16(14) . .
C1B P1B Ni1B 97.74(11) . .
C3B P1B Ni1B 113.93(9) . .
C9B P1B Ni1B 122.05(10) . .
C2B O1B Ni1B 117.5(2) . .
C2B C1B P1B 111.4(2) . .
O1B C2B C1B 125.9(3) . .
C4B C3B C8B 110.5(2) . .
C4B C3B P1B 110.2(2) . .
C8B C3B P1B 113.7(2) . .
C5B C4B C3B 111.3(3) . .
C4B C5B C6B 111.2(3) . .
C7B C6B C5B 110.6(3) . .
C8B C7B C6B 111.6(3) . .
C7B C8B C3B 111.9(2) . .
C14B C9B C10B 111.0(3) . .
C14B C9B P1B 110.7(2) . .
C10B C9B P1B 113.3(2) . .
C11B C10B C9B 111.2(2) . .
C12B C11B C10B 112.1(3) . .
C11B C12B C13B 111.4(3) . .
C12B C13B C14B 111.5(2) . .
C9B C14B C13B 111.0(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1A O1A 1.864(2) 2_766
Ni1A O1A 1.864(2) .
Ni1A P1A 2.2175(8) 2_766
Ni1A P1A 2.2175(8) .
P1A C1A 1.773(3) .
P1A C9A 1.842(3) .
P1A C3A 1.843(3) .
O1A C2A 1.324(4) .
C1A C2A 1.343(4) .
C3A C8A 1.530(4) .
C3A C4A 1.530(4) .
C4A C5A 1.536(5) .
C5A C6A 1.517(4) .
C6A C7A 1.525(5) .
C7A C8A 1.526(5) .
C9A C14A 1.531(4) .
C9A C10A 1.532(4) .
C10A C11A 1.524(4) .
C11A C12A 1.526(4) .
C12A C13A 1.522(5) .
C13A C14A 1.537(4) .
Ni1B O1B 1.866(2) .
Ni1B O1B 1.866(2) 2_565
Ni1B P1B 2.2171(8) .
Ni1B P1B 2.2171(8) 2_565
P1B C1B 1.775(3) .
P1B C3B 1.839(3) .
P1B C9B 1.843(3) .
O1B C2B 1.317(4) .
C1B C2B 1.350(4) .
C3B C4B 1.535(4) .
C3B C8B 1.538(4) .
C4B C5B 1.524(5) .
C5B C6B 1.526(4) .
C6B C7B 1.525(4) .
C7B C8B 1.517(5) .
C9B C14B 1.527(4) .
C9B C10B 1.538(4) .
C10B C11B 1.534(4) .
C11B C12B 1.521(5) .
C12B C13B 1.525(4) .
C13B C14B 1.527(4) .
