#------------------------------------------------------------------------------
#$Date: 2017-03-02 16:12:34 +0100 (jue 02 de mar de 2017) $
#$Revision: 192777 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/05/7000509.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_7000509
loop_
_publ_author_name
'Cloke, F. Geoffrey N.'
'Green, Jennifer C.'
'Hitchcock, Peter B.'
'Nixon, John F.'
'Suter, James L.'
'Wilson, D. James'
_publ_section_title
;
 Syntheses, structural studies, photoelectron spectra and density
 functional theory calculations of the “pseudo”
 tetraphospha-metallocenes [M(η-P2C3But3)2], (M = Ni, Pd, Pt)
;
_journal_issue                   7
_journal_name_full               'Dalton Transactions'
_journal_page_first              1164
_journal_page_last               1171
_journal_paper_doi               10.1039/b815255a
_journal_year                    2009
_chemical_formula_moiety         'C30 H54 Ni P4'
_chemical_formula_sum            'C30 H54 Ni P4'
_chemical_formula_weight         597.32
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 103.84(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.396(4)
_cell_length_b                   9.479(2)
_cell_length_c                   20.102(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     3218.5(17)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta 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  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0790
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5840
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0461
_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)+(0.0334P)²+0.1681P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1056
_reflns_number_gt                4140
_reflns_number_total             5652
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b815255a.txt
_cod_data_source_block           mar999
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_space_group_number' data item was removed -- it should
have been renamed to '_space_group_IT_number' as specified in the
replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst',
but the replacement data item was already present in the data block
and had the same value as the '_symmetry_space_group_number' data
item.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
;
_cod_original_cell_volume        3218.5(16)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7000509
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, 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
Ni Ni 0.21572(3) 0.07794(5) 0.16844(2) 0.01594(13) Uani 1 1 d . . .
P1 P 0.26001(6) -0.05009(9) 0.26703(5) 0.0192(2) Uani 1 1 d . A 2
P2 P 0.16810(5) 0.20064(10) 0.24629(5) 0.0187(2) Uani 1 1 d . A 2
P3 P 0.26537(5) 0.25648(9) 0.11169(5) 0.0187(2) Uani 1 1 d . A 2
P4 P 0.15890(6) 0.01859(10) 0.05108(5) 0.0199(2) Uani 1 1 d . A 2
C1 C 0.1626(2) 0.0146(4) 0.24206(18) 0.0178(8) Uani 1 1 d . A 2
C2 C 0.2649(2) 0.2193(4) 0.31204(17) 0.0184(8) Uani 1 1 d . A 2
C3 C 0.3044(2) 0.0964(4) 0.32610(17) 0.0176(8) Uani 1 1 d . A 2
C4 C 0.0873(2) -0.0754(4) 0.2313(2) 0.0259(9) Uani 1 1 d . A 2
C5 C 0.0719(3) -0.0949(5) 0.3026(2) 0.0450(12) Uani 1 1 d . A 2
H5A H 0.0655 -0.0024 0.3223 0.068 Uiso 1 1 calc R A 2
H5B H 0.1167 -0.1445 0.3321 0.068 Uiso 1 1 calc R A 2
H5C H 0.0235 -0.1505 0.2989 0.068 Uiso 1 1 calc R A 2
C6 C 0.0983(2) -0.2192(4) 0.2010(2) 0.0345(10) Uani 1 1 d . A 2
H6A H 0.0494 -0.2740 0.1952 0.052 Uiso 1 1 calc R A 2
H6B H 0.1418 -0.2694 0.2319 0.052 Uiso 1 1 calc R A 2
H6C H 0.1108 -0.2065 0.1564 0.052 Uiso 1 1 calc R A 2
C7 C 0.0163(2) -0.0034(4) 0.1850(2) 0.0384(11) Uani 1 1 d . A 2
H7A H 0.0083 0.0891 0.2041 0.058 Uiso 1 1 calc R A 2
H7B H -0.0310 -0.0616 0.1818 0.058 Uiso 1 1 calc R A 2
H7C H 0.0259 0.0089 0.1392 0.058 Uiso 1 1 calc R A 2
C8 C 0.2774(2) 0.3730(4) 0.33853(18) 0.0230(8) Uani 1 1 d . A 2
C9 C 0.2237(2) 0.3997(4) 0.3878(2) 0.0349(10) Uani 1 1 d . A 2
H9A H 0.1691 0.3740 0.3653 0.052 Uiso 1 1 calc R A 2
H9B H 0.2259 0.4997 0.4004 0.052 Uiso 1 1 calc R A 2
H9C H 0.2418 0.3422 0.4291 0.052 Uiso 1 1 calc R A 2
C10 C 0.2524(3) 0.4758(4) 0.2776(2) 0.0370(11) Uani 1 1 d . A 2
H10A H 0.1981 0.4545 0.2524 0.056 Uiso 1 1 calc R A 2
H10B H 0.2883 0.4654 0.2470 0.056 Uiso 1 1 calc R A 2
H10C H 0.2550 0.5729 0.2948 0.056 Uiso 1 1 calc R A 2
C11 C 0.3620(2) 0.4153(4) 0.3734(2) 0.0334(10) Uani 1 1 d . A 2
H11A H 0.3963 0.3998 0.3419 0.050 Uiso 1 1 calc R A 2
H11B H 0.3807 0.3580 0.4147 0.050 Uiso 1 1 calc R A 2
H11C H 0.3632 0.5152 0.3861 0.050 Uiso 1 1 calc R A 2
C12 C 0.3747(2) 0.0514(4) 0.38597(19) 0.0254(9) Uani 1 1 d . A 2
C13 C 0.3540(2) 0.0906(4) 0.45398(18) 0.0316(10) Uani 1 1 d . A 2
H13A H 0.3478 0.1931 0.4563 0.047 Uiso 1 1 calc R A 2
H13B H 0.3966 0.0594 0.4924 0.047 Uiso 1 1 calc R A 2
H13C H 0.3044 0.0442 0.4565 0.047 Uiso 1 1 calc R A 2
C14 C 0.3846(2) -0.1103(4) 0.3884(2) 0.0338(10) Uani 1 1 d . A 2
H14A H 0.3979 -0.1429 0.3462 0.051 Uiso 1 1 calc R A 2
H14B H 0.3350 -0.1544 0.3925 0.051 Uiso 1 1 calc R A 2
H14C H 0.4271 -0.1364 0.4279 0.051 Uiso 1 1 calc R A 2
C15 C 0.4560(2) 0.1091(5) 0.3817(2) 0.0365(11) Uani 1 1 d . A 2
H15A H 0.4670 0.0809 0.3380 0.055 Uiso 1 1 calc R A 2
H15B H 0.4970 0.0709 0.4196 0.055 Uiso 1 1 calc R A 2
H15C H 0.4557 0.2123 0.3847 0.055 Uiso 1 1 calc R A 2
C16 C 0.1695(2) 0.1972(4) 0.07116(18) 0.0197(8) Uani 1 1 d . A 2
C17 C 0.2605(2) -0.0273(4) 0.08817(17) 0.0167(7) Uani 1 1 d . A 2
C18 C 0.31138(19) 0.0866(4) 0.11785(17) 0.0162(7) Uani 1 1 d . A 2
C19 C 0.1023(2) 0.3043(4) 0.04691(19) 0.0226(8) Uani 1 1 d . A 2
C20 C 0.1107(3) 0.3557(4) -0.0236(2) 0.0363(10) Uani 1 1 d . A 2
H20A H 0.1635 0.3961 -0.0191 0.054 Uiso 1 1 calc R A 2
H20B H 0.0705 0.4278 -0.0410 0.054 Uiso 1 1 calc R A 2
H20C H 0.1033 0.2761 -0.0555 0.054 Uiso 1 1 calc R A 2
C21 C 0.0205(2) 0.2403(5) 0.0394(3) 0.0446(12) Uani 1 1 d . A 2
H21A H 0.0149 0.2074 0.0842 0.067 Uiso 1 1 calc R A 2
H21B H 0.0140 0.1605 0.0075 0.067 Uiso 1 1 calc R A 2
H21C H -0.0199 0.3117 0.0216 0.067 Uiso 1 1 calc R A 2
C22 C 0.1095(2) 0.4315(4) 0.0953(2) 0.0320(10) Uani 1 1 d . A 2
H22A H 0.1617 0.4751 0.1006 0.048 Uiso 1 1 calc R A 2
H22B H 0.1031 0.4000 0.1401 0.048 Uiso 1 1 calc R A 2
H22C H 0.0682 0.5005 0.0760 0.048 Uiso 1 1 calc R A 2
C23 C 0.2804(2) -0.1852(4) 0.07561(19) 0.0237(9) Uani 1 1 d . A 2
C24 C 0.2992(2) -0.2772(4) 0.1406(2) 0.0294(9) Uani 1 1 d . A 2
H24A H 0.2556 -0.2708 0.1636 0.044 Uiso 1 1 calc R A 2
H24B H 0.3481 -0.2437 0.1716 0.044 Uiso 1 1 calc R A 2
H24C H 0.3059 -0.3755 0.1280 0.044 Uiso 1 1 calc R A 2
C25 C 0.2099(2) -0.2582(4) 0.0267(2) 0.0342(10) Uani 1 1 d . A 2
H25A H 0.1949 -0.2047 -0.0162 0.051 Uiso 1 1 calc R A 2
H25B H 0.1649 -0.2623 0.0481 0.051 Uiso 1 1 calc R A 2
H25C H 0.2251 -0.3542 0.0169 0.051 Uiso 1 1 calc R A 2
C26 C 0.3481(2) -0.1926(4) 0.0388(2) 0.0299(9) Uani 1 1 d . A 2
H26A H 0.3352 -0.1334 -0.0024 0.045 Uiso 1 1 calc R A 2
H26B H 0.3552 -0.2905 0.0257 0.045 Uiso 1 1 calc R A 2
H26C H 0.3971 -0.1587 0.0695 0.045 Uiso 1 1 calc R A 2
C27 C 0.4029(2) 0.0960(4) 0.14924(18) 0.0191(8) Uani 1 1 d . A 2
C28 C 0.4442(2) 0.1222(4) 0.09049(19) 0.0286(9) Uani 1 1 d . A 2
H28A H 0.4203 0.2043 0.0638 0.043 Uiso 1 1 calc R A 2
H28B H 0.4378 0.0390 0.0607 0.043 Uiso 1 1 calc R A 2
H28C H 0.5007 0.1398 0.1096 0.043 Uiso 1 1 calc R A 2
C29 C 0.4397(2) -0.0314(4) 0.19191(19) 0.0258(9) Uani 1 1 d . A 2
H29A H 0.4290 -0.1169 0.1638 0.039 Uiso 1 1 calc R A 2
H29B H 0.4167 -0.0412 0.2316 0.039 Uiso 1 1 calc R A 2
H29C H 0.4971 -0.0177 0.2076 0.039 Uiso 1 1 calc R A 2
C30 C 0.4231(2) 0.2229(4) 0.19765(19) 0.0259(9) Uani 1 1 d . A 2
H30A H 0.4011 0.3090 0.1733 0.039 Uiso 1 1 calc R A 2
H30B H 0.4807 0.2320 0.2132 0.039 Uiso 1 1 calc R A 2
H30C H 0.4003 0.2089 0.2373 0.039 Uiso 1 1 calc R A 2
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'
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'
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
C1 Ni C18 154.42(14) . . ?
C1 Ni C17 135.32(13) . . ?
C18 Ni C17 38.52(12) . . ?
C1 Ni C16 131.38(14) . . ?
C18 Ni C16 73.99(13) . . ?
C17 Ni C16 72.73(13) . . ?
C1 Ni P2 48.42(10) . . ?
C18 Ni P2 139.59(10) . . ?
C17 Ni P2 175.81(9) . . ?
C16 Ni P2 103.33(10) . . ?
C1 Ni P1 47.61(10) . . ?
C18 Ni P1 106.92(10) . . ?
C17 Ni P1 106.86(9) . . ?
C16 Ni P1 178.08(10) . . ?
P2 Ni P1 77.12(4) . . ?
C1 Ni P3 150.32(10) . . ?
C18 Ni P3 47.00(9) . . ?
C17 Ni P3 74.36(9) . . ?
C16 Ni P3 45.53(9) . . ?
P2 Ni P3 101.91(4) . . ?
P1 Ni P3 136.31(4) . . ?
C1 Ni P4 119.97(11) . . ?
C18 Ni P4 74.15(10) . . ?
C17 Ni P4 45.91(9) . . ?
C16 Ni P4 43.96(10) . . ?
P2 Ni P4 132.00(4) . . ?
P1 Ni P4 134.46(4) . . ?
P3 Ni P4 78.55(4) . . ?
C1 P1 C3 98.37(16) . . ?
C1 P1 Ni 57.82(11) . . ?
C3 P1 Ni 99.10(11) . . ?
C1 P2 C2 99.00(16) . . ?
C1 P2 Ni 58.50(11) . . ?
C2 P2 Ni 96.90(11) . . ?
C16 P3 C18 95.93(16) . . ?
C16 P3 Ni 64.70(12) . . ?
C18 P3 Ni 61.48(11) . . ?
C16 P4 C17 95.76(16) . . ?
C16 P4 Ni 63.09(12) . . ?
C17 P4 Ni 61.05(11) . . ?
C4 C1 P1 125.4(3) . . ?
C4 C1 P2 126.5(3) . . ?
P1 C1 P2 107.29(19) . . ?
C4 C1 Ni 126.0(2) . . ?
P1 C1 Ni 74.57(13) . . ?
P2 C1 Ni 73.08(13) . . ?
C3 C2 C8 135.9(3) . . ?
C3 C2 P2 113.0(3) . . ?
C8 C2 P2 111.0(2) . . ?
C2 C3 C12 131.7(3) . . ?
C2 C3 P1 113.4(3) . . ?
C12 C3 P1 114.6(2) . . ?
C7 C4 C6 108.6(3) . . ?
C7 C4 C5 109.3(3) . . ?
C6 C4 C5 109.4(3) . . ?
C7 C4 C1 112.2(3) . . ?
C6 C4 C1 111.6(3) . . ?
C5 C4 C1 105.6(3) . . ?
C11 C8 C9 109.2(3) . . ?
C11 C8 C10 104.9(3) . . ?
C9 C8 C10 107.9(3) . . ?
C11 C8 C2 116.5(3) . . ?
C9 C8 C2 108.6(3) . . ?
C10 C8 C2 109.3(3) . . ?
C15 C12 C13 112.2(3) . . ?
C15 C12 C14 105.0(3) . . ?
C13 C12 C14 105.0(3) . . ?
C15 C12 C3 115.0(3) . . ?
C13 C12 C3 108.2(3) . . ?
C14 C12 C3 110.9(3) . . ?
C19 C16 P4 122.6(3) . . ?
C19 C16 P3 120.0(3) . . ?
P4 C16 P3 116.9(2) . . ?
C19 C16 Ni 134.3(3) . . ?
P4 C16 Ni 72.95(13) . . ?
P3 C16 Ni 69.77(12) . . ?
C18 C17 C23 130.4(3) . . ?
C18 C17 P4 116.0(2) . . ?
C23 C17 P4 113.3(2) . . ?
C18 C17 Ni 69.11(19) . . ?
C23 C17 Ni 133.1(2) . . ?
P4 C17 Ni 73.04(12) . . ?
C17 C18 C27 132.6(3) . . ?
C17 C18 P3 115.3(2) . . ?
C27 C18 P3 111.8(2) . . ?
C17 C18 Ni 72.37(19) . . ?
C27 C18 Ni 129.6(2) . . ?
P3 C18 Ni 71.52(12) . . ?
C21 C19 C22 108.0(3) . . ?
C21 C19 C16 113.0(3) . . ?
C22 C19 C16 112.2(3) . . ?
C21 C19 C20 109.1(3) . . ?
C22 C19 C20 108.8(3) . . ?
C16 C19 C20 105.6(3) . . ?
C26 C23 C24 110.5(3) . . ?
C26 C23 C25 104.8(3) . . ?
C24 C23 C25 105.2(3) . . ?
C26 C23 C17 110.2(3) . . ?
C24 C23 C17 114.4(3) . . ?
C25 C23 C17 111.1(3) . . ?
C29 C27 C30 105.2(3) . . ?
C29 C27 C28 110.3(3) . . ?
C30 C27 C28 106.4(3) . . ?
C29 C27 C18 115.4(3) . . ?
C30 C27 C18 110.9(3) . . ?
C28 C27 C18 108.4(3) . . ?
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
Ni C1 2.014(3) . ?
Ni C18 2.149(3) . ?
Ni C17 2.193(3) . ?
Ni C16 2.235(4) . ?
Ni P2 2.2601(12) . ?
Ni P1 2.2942(12) . ?
Ni P3 2.3201(11) . ?
Ni P4 2.3967(14) . ?
P1 C1 1.758(4) . ?
P1 C3 1.869(4) . ?
P2 C1 1.767(4) . ?
P2 C2 1.884(4) . ?
P3 C16 1.764(4) . ?
P3 C18 1.789(3) . ?
P4 C16 1.740(4) . ?
P4 C17 1.800(4) . ?
C1 C4 1.536(5) . ?
C2 C3 1.348(5) . ?
C2 C8 1.548(5) . ?
C3 C12 1.556(5) . ?
C4 C7 1.518(5) . ?
C4 C6 1.523(5) . ?
C4 C5 1.531(5) . ?
C8 C11 1.524(5) . ?
C8 C9 1.537(5) . ?
C8 C10 1.544(5) . ?
C12 C15 1.537(5) . ?
C12 C13 1.540(5) . ?
C12 C14 1.542(5) . ?
C16 C19 1.537(5) . ?
C17 C18 1.433(5) . ?
C17 C23 1.570(5) . ?
C18 C27 1.568(5) . ?
C19 C21 1.520(5) . ?
C19 C22 1.535(5) . ?
C19 C20 1.538(5) . ?
C23 C26 1.535(5) . ?
C23 C24 1.539(5) . ?
C23 C25 1.540(5) . ?
C27 C29 1.531(5) . ?
C27 C30 1.534(5) . ?
C27 C28 1.542(5) . ?
