#------------------------------------------------------------------------------
#$Date: 2016-03-26 01:54:20 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180114 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/12/7101204.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_7101204
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            'C56 H56 Ni P4'
_chemical_formula_weight         911.60
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.142(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.9448(4)
_cell_length_b                   11.8350(3)
_cell_length_c                   20.0660(4)
_cell_measurement_temperature    183(2)
_cell_volume                     4669.79(18)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            9633
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         5338
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0329
_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)+(0.0420P)²+2.5743P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0857
_reflns_number_gt                4257
_reflns_number_total             5338
_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               7101204
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 0.95551(2) 0.7500 0.01985(9) Uani 1 2 d S
P1 P 0.07778(2) 1.04944(4) 0.72139(2) 0.02380(11) Uani 1 1 d .
P2 P -0.04523(2) 0.83862(3) 0.66037(2) 0.02231(10) Uani 1 1 d .
C1 C 0.11104(8) 0.96967(15) 0.66090(8) 0.0293(4) Uani 1 1 d .
H1A H 0.1503 1.0104 0.6556 0.035 Uiso 1 1 calc R
H1B H 0.1268 0.8943 0.6813 0.035 Uiso 1 1 calc R
C2 C 0.05478(9) 0.95599(15) 0.58725(8) 0.0307(4) Uani 1 1 d .
H2A H 0.0145 1.0001 0.5868 0.037 Uiso 1 1 calc R
H2B H 0.0713 0.9887 0.5508 0.037 Uiso 1 1 calc R
C3 C 0.03283(9) 0.83428(15) 0.56671(9) 0.0317(4) Uani 1 1 d .
H3A H 0.0709 0.7943 0.5584 0.038 Uiso 1 1 calc R
H3B H -0.0057 0.8353 0.5211 0.038 Uiso 1 1 calc R
C4 C 0.01130(8) 0.76555(15) 0.62022(8) 0.0283(3) Uani 1 1 d .
H4A H 0.0529 0.7413 0.6590 0.034 Uiso 1 1 calc R
H4B H -0.0121 0.6964 0.5962 0.034 Uiso 1 1 calc R
C5 C 0.15892(8) 1.10078(15) 0.78754(9) 0.0303(4) Uani 1 1 d .
C6 C 0.16417(10) 1.20985(17) 0.81454(10) 0.0417(5) Uani 1 1 d .
H6A H 0.1269 1.2603 0.7961 0.050 Uiso 1 1 calc R
C7 C 0.22263(11) 1.2469(2) 0.86785(12) 0.0555(6) Uani 1 1 d .
H7A H 0.2250 1.3219 0.8855 0.067 Uiso 1 1 calc R
C8 C 0.27687(11) 1.1751(2) 0.89486(12) 0.0556(6) Uani 1 1 d .
H8A H 0.3165 1.1995 0.9320 0.067 Uiso 1 1 calc R
C9 C 0.27344(10) 1.0681(2) 0.86797(11) 0.0491(5) Uani 1 1 d .
H9A H 0.3112 1.0187 0.8861 0.059 Uiso 1 1 calc R
C10 C 0.21508(9) 1.03098(17) 0.81437(10) 0.0385(4) Uani 1 1 d .
H10A H 0.2137 0.9567 0.7959 0.046 Uiso 1 1 calc R
C11 C 0.05423(9) 1.18143(15) 0.66838(9) 0.0314(4) Uani 1 1 d .
C12 C -0.00956(10) 1.22719(16) 0.65411(9) 0.0381(4) Uani 1 1 d .
H12A H -0.0402 1.1919 0.6732 0.046 Uiso 1 1 calc R
C13 C -0.03037(13) 1.32362(18) 0.61253(11) 0.0522(6) Uani 1 1 d .
H13A H -0.0747 1.3534 0.6033 0.063 Uiso 1 1 calc R
C14 C 0.01385(15) 1.37543(18) 0.58496(12) 0.0601(7) Uani 1 1 d .
H14A H 0.0003 1.4417 0.5569 0.072 Uiso 1 1 calc R
C15 C 0.07769(14) 1.33107(19) 0.59812(12) 0.0567(6) Uani 1 1 d .
H15A H 0.1081 1.3665 0.5787 0.068 Uiso 1 1 calc R
C16 C 0.09788(11) 1.23527(19) 0.63940(11) 0.0469(5) Uani 1 1 d .
H16A H 0.1422 1.2056 0.6482 0.056 Uiso 1 1 calc R
C17 C -0.08903(8) 0.71561(14) 0.68193(8) 0.0272(3) Uani 1 1 d .
C18 C -0.14662(9) 0.73685(16) 0.69954(9) 0.0327(4) Uani 1 1 d .
H18A H -0.1639 0.8117 0.6956 0.039 Uiso 1 1 calc R
C19 C -0.17957(10) 0.65201(17) 0.72271(9) 0.0389(4) Uani 1 1 d .
H19A H -0.2191 0.6689 0.7339 0.047 Uiso 1 1 calc R
C20 C -0.15473(11) 0.54273(17) 0.72948(11) 0.0446(5) Uani 1 1 d .
H20A H -0.1763 0.4843 0.7464 0.054 Uiso 1 1 calc R
C21 C -0.09852(12) 0.51999(17) 0.71146(12) 0.0492(5) Uani 1 1 d .
H21A H -0.0813 0.4451 0.7159 0.059 Uiso 1 1 calc R
C22 C -0.06632(10) 0.60481(15) 0.68683(10) 0.0390(4) Uani 1 1 d .
H22A H -0.0284 0.5866 0.6732 0.047 Uiso 1 1 calc R
C23 C -0.11383(8) 0.88379(15) 0.57876(8) 0.0265(3) Uani 1 1 d .
C24 C -0.15108(9) 0.80570(17) 0.52814(9) 0.0374(4) Uani 1 1 d .
H24A H -0.1411 0.7274 0.5354 0.045 Uiso 1 1 calc R
C25 C -0.20272(10) 0.8416(2) 0.46725(10) 0.0456(5) Uani 1 1 d .
H25A H -0.2273 0.7880 0.4327 0.055 Uiso 1 1 calc R
C26 C -0.21817(10) 0.9547(2) 0.45701(10) 0.0465(5) Uani 1 1 d .
H26A H -0.2541 0.9791 0.4159 0.056 Uiso 1 1 calc R
C27 C -0.18152(10) 1.03270(19) 0.50641(10) 0.0442(5) Uani 1 1 d .
H27A H -0.1918 1.1109 0.4990 0.053 Uiso 1 1 calc R
C28 C -0.12951(9) 0.99717(16) 0.56713(9) 0.0332(4) Uani 1 1 d .
H28A H -0.1045 1.0514 0.6010 0.040 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'
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 119.46(2) . 2_556
P1 Ni P2 104.600(15) . .
P1 Ni P2 112.318(15) 2_556 .
P1 Ni P2 112.320(15) . 2_556
P1 Ni P2 104.599(15) 2_556 2_556
P2 Ni P2 102.38(2) . 2_556
C1 P1 C11 97.99(8) . .
C1 P1 C5 100.17(8) . .
C11 P1 C5 97.53(8) . .
C1 P1 Ni 113.07(6) . .
C11 P1 Ni 119.90(6) . .
C5 P1 Ni 123.62(5) . .
C23 P2 C17 97.94(7) . .
C23 P2 C4 99.64(7) . .
C17 P2 C4 100.16(8) . .
C23 P2 Ni 121.71(6) . .
C17 P2 Ni 114.27(5) . .
C4 P2 Ni 119.08(5) . .
C2 C1 P1 110.13(11) . .
C3 C2 C1 114.58(14) . .
C2 C3 C4 116.48(14) . .
C3 C4 P2 116.20(12) . .
C10 C5 C6 117.38(17) . .
C10 C5 P1 121.79(14) . .
C6 C5 P1 120.75(14) . .
C5 C6 C7 121.6(2) . .
C8 C7 C6 119.9(2) . .
C9 C8 C7 119.57(19) . .
C8 C9 C10 120.6(2) . .
C5 C10 C9 120.9(2) . .
C12 C11 C16 117.50(18) . .
C12 C11 P1 119.79(14) . .
C16 C11 P1 122.66(16) . .
C11 C12 C13 121.88(19) . .
C14 C13 C12 119.4(2) . .
C15 C14 C13 119.8(2) . .
C14 C15 C16 120.3(2) . .
C15 C16 C11 121.0(2) . .
C22 C17 C18 117.32(16) . .
C22 C17 P2 125.11(14) . .
C18 C17 P2 117.40(13) . .
C19 C18 C17 121.97(18) . .
C20 C19 C18 119.76(18) . .
C21 C20 C19 119.05(18) . .
C20 C21 C22 121.12(19) . .
C17 C22 C21 120.73(19) . .
C28 C23 C24 118.63(15) . .
C28 C23 P2 119.85(13) . .
C24 C23 P2 121.51(14) . .
C25 C24 C23 120.53(19) . .
C26 C25 C24 120.00(19) . .
C27 C26 C25 120.00(17) . .
C26 C27 C28 120.13(19) . .
C23 C28 C27 120.69(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni P1 2.2054(4) .
Ni P1 2.2054(4) 2_556
Ni P2 2.2073(4) .
Ni P2 2.2074(4) 2_556
P1 C1 1.8524(17) .
P1 C11 1.8583(18) .
P1 C5 1.8616(17) .
P2 C23 1.8471(15) .
P2 C17 1.8497(17) .
P2 C4 1.8591(16) .
C1 C2 1.549(2) .
C2 C3 1.525(3) .
C3 C4 1.533(2) .
C5 C10 1.385(3) .
C5 C6 1.390(3) .
C6 C7 1.391(3) .
C7 C8 1.372(3) .
C8 C9 1.369(3) .
C9 C10 1.392(3) .
C11 C12 1.377(3) .
C11 C16 1.395(3) .
C12 C13 1.392(3) .
C13 C14 1.376(3) .
C14 C15 1.375(4) .
C15 C16 1.382(3) .
C17 C22 1.387(3) .
C17 C18 1.392(2) .
C18 C19 1.386(3) .
C19 C20 1.383(3) .
C20 C21 1.372(3) .
C21 C22 1.392(3) .
C23 C28 1.382(3) .
C23 C24 1.396(2) .
C24 C25 1.390(3) .
C25 C26 1.376(3) .
C26 C27 1.378(3) .
C27 C28 1.391(2) .
