#------------------------------------------------------------------------------
#$Date: 2016-03-26 01:54:20 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180114 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/12/7101203.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_7101203
loop_
_publ_author_name
'Dirk Walther'
'Reinald Fischer'
'Helmar Gorls'
'Jens Langer'
'Astrid Malassa'
'Gavin Vaughan'
_publ_section_title
;
A Key Step of the Formation of Acrylic Acid from CO₂ and
Ethylene: The Transformation of a Nickelalactone into a
Nickel-acrylate Complex
;
_journal_issue                   23
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/b603540j
_journal_year                    2006
_chemical_formula_sum            'C54 H52 Ni P4'
_chemical_formula_weight         883.55
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.690(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.1812(6)
_cell_length_b                   13.2156(5)
_cell_length_c                   19.9132(4)
_cell_measurement_temperature    183(2)
_cell_volume                     4504.9(2)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_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  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0542
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8793
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.20
_exptl_absorpt_coefficient_mu    0.609
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         5093
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0324P)²+4.0135P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0840
_reflns_number_gt                4239
_reflns_number_total             5093
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b603540j.txt
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'NONE' changed to 'none' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7101203
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Ni Ni 0.0000 -0.00329(2) 0.2500 0.01378(10) Uani 1 2 d S
P1 P -0.04456(3) -0.10201(4) 0.15771(2) 0.01577(12) Uani 1 1 d .
P2 P 0.08861(3) 0.07840(4) 0.22050(2) 0.01678(12) Uani 1 1 d .
C1 C 0.02497(11) -0.13103(16) 0.11061(10) 0.0218(4) Uani 1 1 d .
H1B H 0.0628(13) -0.1790(17) 0.1407(11) 0.028(6) Uiso 1 1 d .
H1A H -0.0031(13) -0.1645(16) 0.0668(11) 0.029(6) Uiso 1 1 d .
C2 C 0.06756(12) -0.03873(17) 0.09668(10) 0.0233(4) Uani 1 1 d .
H2B H 0.0306(12) 0.0142(16) 0.0727(11) 0.025(6) Uiso 1 1 d .
H2A H 0.0914(13) -0.0556(17) 0.0631(11) 0.029(6) Uiso 1 1 d .
C3 C 0.13017(11) 0.00215(16) 0.16392(10) 0.0222(4) Uani 1 1 d .
H3B H 0.1571(12) -0.0549(17) 0.1934(11) 0.027(6) Uiso 1 1 d .
H3A H 0.1689(13) 0.0415(17) 0.1521(11) 0.027(6) Uiso 1 1 d .
C4 C -0.12825(10) -0.05963(15) 0.08081(9) 0.0184(4) Uani 1 1 d .
C5 C -0.17959(13) -0.12569(18) 0.03273(11) 0.0315(5) Uani 1 1 d .
H5 H -0.1727(13) -0.1959(19) 0.0391(11) 0.034(6) Uiso 1 1 d .
C6 C -0.24106(13) -0.08884(19) -0.02457(12) 0.0368(6) Uani 1 1 d .
H6 H -0.2732(15) -0.134(2) -0.0587(14) 0.050(7) Uiso 1 1 d .
C7 C -0.25166(12) 0.01406(18) -0.03481(11) 0.0311(5) Uani 1 1 d .
H7 H -0.2944(14) 0.0400(18) -0.0737(12) 0.038(6) Uiso 1 1 d .
C8 C -0.20080(12) 0.08041(17) 0.01168(10) 0.0262(4) Uani 1 1 d .
H8 H -0.2077(14) 0.156(2) 0.0062(12) 0.042(7) Uiso 1 1 d .
C9 C -0.13973(11) 0.04314(16) 0.06907(10) 0.0221(4) Uani 1 1 d .
H9 H -0.1077(13) 0.0903(17) 0.1012(11) 0.029(6) Uiso 1 1 d .
C10 C -0.07692(10) -0.23021(14) 0.17086(9) 0.0182(4) Uani 1 1 d .
C11 C -0.13472(12) -0.23918(16) 0.20214(10) 0.0235(4) Uani 1 1 d .
H11 H -0.1565(12) -0.1812(17) 0.2123(10) 0.026(6) Uiso 1 1 d .
C12 C -0.15942(13) -0.33260(17) 0.21763(10) 0.0293(5) Uani 1 1 d .
H12 H -0.1966(16) -0.338(2) 0.2398(14) 0.056(8) Uiso 1 1 d .
C13 C -0.12607(13) -0.41965(17) 0.20299(11) 0.0318(5) Uani 1 1 d .
H13 H -0.1409(13) -0.4800(18) 0.2143(11) 0.032(6) Uiso 1 1 d .
C14 C -0.06902(13) -0.41313(17) 0.17178(11) 0.0310(5) Uani 1 1 d .
H14 H -0.0462(14) -0.472(2) 0.1621(12) 0.042(7) Uiso 1 1 d .
C15 C -0.04514(12) -0.31920(16) 0.15515(10) 0.0257(4) Uani 1 1 d .
H15 H -0.0049(14) -0.3171(18) 0.1356(12) 0.038(6) Uiso 1 1 d .
C16 C 0.06216(11) 0.19322(15) 0.16351(10) 0.0229(4) Uani 1 1 d .
C17 C 0.10884(15) 0.23190(18) 0.12636(12) 0.0365(5) Uani 1 1 d .
H17 H 0.1569(14) 0.2032(18) 0.1324(11) 0.035(6) Uiso 1 1 d .
C18 C 0.08397(18) 0.3136(2) 0.08024(14) 0.0488(7) Uani 1 1 d .
H18 H 0.1150(15) 0.336(2) 0.0534(14) 0.055(8) Uiso 1 1 d .
C19 C 0.01245(18) 0.3577(2) 0.07081(14) 0.0501(7) Uani 1 1 d .
H19 H -0.0054(16) 0.411(2) 0.0405(14) 0.055(8) Uiso 1 1 d .
C20 C -0.03383(16) 0.32181(18) 0.10796(13) 0.0413(6) Uani 1 1 d .
H20 H -0.0825(16) 0.349(2) 0.1019(13) 0.048(7) Uiso 1 1 d .
C21 C -0.00870(12) 0.24022(16) 0.15400(11) 0.0275(5) Uani 1 1 d .
H21 H -0.0398(12) 0.2143(16) 0.1790(11) 0.024(5) Uiso 1 1 d .
C22 C 0.18090(11) 0.12254(15) 0.28760(9) 0.0206(4) Uani 1 1 d .
C23 C 0.19436(12) 0.22438(17) 0.30662(11) 0.0258(4) Uani 1 1 d .
H23 H 0.1579(13) 0.2700(17) 0.2845(11) 0.026(6) Uiso 1 1 d .
C24 C 0.26313(14) 0.25396(19) 0.35945(11) 0.0330(5) Uani 1 1 d .
H24 H 0.2682(14) 0.322(2) 0.3689(12) 0.044(7) Uiso 1 1 d .
C25 C 0.31911(13) 0.18407(19) 0.39367(11) 0.0355(5) Uani 1 1 d .
H25 H 0.3664(15) 0.2036(19) 0.4300(13) 0.047(7) Uiso 1 1 d .
C26 C 0.30670(13) 0.08310(19) 0.37565(11) 0.0333(5) Uani 1 1 d .
H26 H 0.3442(15) 0.033(2) 0.3986(13) 0.044(7) Uiso 1 1 d .
C27 C 0.23804(11) 0.05247(17) 0.32353(10) 0.0248(4) Uani 1 1 d .
H27 H 0.2273(12) -0.0197(18) 0.3122(11) 0.029(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'
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
P1 Ni P1 106.30(3) . 2
P1 Ni P2 115.236(17) . 2
P1 Ni P2 99.681(17) 2 2
P1 Ni P2 99.681(17) . .
P1 Ni P2 115.235(17) 2 .
P2 Ni P2 120.57(3) 2 .
C10 P1 C4 100.58(8) . .
C10 P1 C1 100.78(9) . .
C4 P1 C1 98.95(9) . .
C10 P1 Ni 118.53(6) . .
C4 P1 Ni 119.17(6) . .
C1 P1 Ni 115.40(6) . .
C3 P2 C22 98.86(9) . .
C3 P2 C16 98.48(9) . .
C22 P2 C16 99.70(9) . .
C3 P2 Ni 112.64(7) . .
C22 P2 Ni 122.29(6) . .
C16 P2 Ni 120.44(6) . .
C2 C1 P1 113.79(14) . .
C1 C2 C3 113.41(16) . .
C2 C3 P2 112.81(13) . .
C9 C4 C5 118.08(17) . .
C9 C4 P1 118.30(14) . .
C5 C4 P1 123.60(15) . .
C6 C5 C4 120.8(2) . .
C7 C6 C5 120.1(2) . .
C6 C7 C8 119.92(19) . .
C7 C8 C9 119.7(2) . .
C4 C9 C8 121.43(18) . .
C15 C10 C11 117.43(18) . .
C15 C10 P1 124.68(15) . .
C11 C10 P1 117.81(15) . .
C12 C11 C10 121.7(2) . .
C13 C12 C11 119.9(2) . .
C12 C13 C14 119.7(2) . .
C13 C14 C15 120.3(2) . .
C14 C15 C10 120.9(2) . .
C21 C16 C17 117.82(19) . .
C21 C16 P2 119.16(15) . .
C17 C16 P2 122.93(16) . .
C18 C17 C16 120.9(2) . .
C19 C18 C17 120.0(2) . .
C20 C19 C18 120.0(2) . .
C19 C20 C21 119.8(2) . .
C16 C21 C20 121.5(2) . .
C23 C22 C27 117.91(18) . .
C23 C22 P2 122.16(15) . .
C27 C22 P2 119.85(15) . .
C22 C23 C24 120.4(2) . .
C25 C24 C23 120.9(2) . .
C24 C25 C26 119.5(2) . .
C25 C26 C27 120.2(2) . .
C26 C27 C22 121.1(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni P1 2.1754(5) .
Ni P1 2.1755(5) 2
Ni P2 2.1780(5) 2
Ni P2 2.1781(5) .
P1 C10 1.8409(19) .
P1 C4 1.8449(18) .
P1 C1 1.8503(19) .
P2 C3 1.8519(19) .
P2 C22 1.8521(19) .
P2 C16 1.858(2) .
C1 C2 1.520(3) .
C2 C3 1.534(3) .
C4 C9 1.382(3) .
C4 C5 1.396(3) .
C5 C6 1.389(3) .
C6 C7 1.379(3) .
C7 C8 1.380(3) .
C8 C9 1.388(3) .
C10 C15 1.392(3) .
C10 C11 1.395(3) .
C11 C12 1.384(3) .
C12 C13 1.377(3) .
C13 C14 1.380(3) .
C14 C15 1.391(3) .
C16 C21 1.385(3) .
C16 C17 1.397(3) .
C17 C18 1.390(3) .
C18 C19 1.379(4) .
C19 C20 1.378(4) .
C20 C21 1.389(3) .
C22 C23 1.397(3) .
C22 C27 1.396(3) .
C23 C24 1.392(3) .
C24 C25 1.373(3) .
C25 C26 1.381(3) .
C26 C27 1.388(3) .
