#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/20/2012029.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2012029
loop_
_publ_author_name
'Davison, Jo C.'
'Foreman, Mark R. St.-J.'
'Howie, R. Alan'
'Plater, M. John'
'Skakle, Janet M.S.'
_publ_section_title
;
 A new polymorph, form C, of
 [1,2-bis(diphenylphosphino)ethane]dichloronickel(II)
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              690
_journal_page_last               693
_journal_paper_doi               10.1107/S0108270101003961
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          '[NiCl2 (C26 H24 P2)]'
_chemical_formula_moiety         'C26 H24 Cl2 Ni P2'
_chemical_formula_sum            'C26 H24 Cl2 Ni P2'
_chemical_formula_weight         528.0
_chemical_name_systematic
;
Dichloro[1,2-bis(diphenylphosphino)ethane]nickel(II) (form C at 150 K)
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'I 2y'
_symmetry_space_group_name_H-M   'I 1 2 1'
_audit_creation_method           SHELXL97
_cell_angle_alpha                90
_cell_angle_beta                 105.983(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.4551(14)
_cell_length_b                   7.9901(8)
_cell_length_c                   13.0350(19)
_cell_measurement_reflns_used    5686
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     1247.1(3)
_computing_cell_refinement       'DENZO and COLLECT'
_computing_data_collection
'DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_data_reduction        'DENZO and COLLECT'
_computing_molecular_graphics    'Ortep3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full .492
_diffrn_measured_fraction_theta_max .492
_diffrn_measurement_device_type  Kappa-CCD
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enraf Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .064
_diffrn_reflns_av_sigmaI/netI    .099
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5686
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.0
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.132
_exptl_absorpt_correction_T_max  .999
_exptl_absorpt_correction_T_min  .887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995, 1997)'
_exptl_crystal_colour            brown_yellow
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             544
_exptl_crystal_size_max          .20
_exptl_crystal_size_mid          .03
_exptl_crystal_size_min          .03
_refine_diff_density_max         .54
_refine_diff_density_min         -.58
_refine_ls_abs_structure_details '(Flack, 1983)'
_refine_ls_abs_structure_Flack   .01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2686
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          .084
_refine_ls_R_factor_gt           .050
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0296P)²+0.0327P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .105
_reflns_number_gt                1946
_reflns_number_total             2686
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            gg1036.cif
_cod_data_source_block           C(150)
_cod_original_sg_symbol_H-M      'I 2'
_cod_database_code               2012029
_cod_database_fobs_code          2012029
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Ni .0000 .00232(10) .0000 .0292(2) Uani d S 1 . . Ni
Cl -.12373(12) .18440(10) .02446(11) .0361(4) Uani d . 1 . . Cl
P -.11397(13) -.19118(12) .01230(11) .0328(4) Uani d . 1 . . P
C1 -.0589(4) -.3925(5) -.0186(5) .0511(15) Uani d . 1 . . C
H1A -.0895 -.4844 .0159 .061 Uiso calc R 1 . . H
H1B -.0823 -.4114 -.0967 .061 Uiso calc R 1 . . H
C2 -.1253(4) -.2100(5) .1465(4) .0335(11) Uani d . 1 . . C
C3 -.0519(4) -.1211(6) .2281(4) .0381(11) Uani d . 1 . . C
H3 .0042 -.0532 .2125 .046 Uiso calc R 1 . . H
C4 -.0598(4) -.1304(6) .3316(4) .0463(13) Uani d . 1 . . C
H4 -.0094 -.0685 .3864 .056 Uiso calc R 1 . . H
C5 -.1396(5) -.2279(6) .3558(4) .0466(13) Uani d . 1 . . C
H5 -.1455 -.2325 .4268 .056 Uiso calc R 1 . . H
C6 -.2112(4) -.3190(7) .2765(4) .0485(13) Uani d . 1 . . C
H6 -.2664 -.3876 .2931 .058 Uiso calc R 1 . . H
C7 -.2036(4) -.3118(6) .1727(4) .0479(14) Uani d . 1 . . C
H7 -.2526 -.3773 .1189 .058 Uiso calc R 1 . . H
C8 -.2531(4) -.1743(5) -.0763(4) .0377(12) Uani d . 1 . . C
C9 -.3384(4) -.1065(7) -.0432(4) .0533(14) Uani d . 1 . . C
H9 -.3254 -.0718 .0289 .064 Uiso calc R 1 . . H
C10 -.4453(5) -.0874(7) -.1145(4) .0659(17) Uani d . 1 . . C
H10 -.5042 -.0402 -.0907 .079 Uiso calc R 1 . . H
C11 -.4641(5) -.1373(7) -.2190(5) .0574(15) Uani d . 1 . . C
H11 -.5363 -.1259 -.2674 .069 Uiso calc R 1 . . H
C12 -.3795(6) -.2026(7) -.2529(5) .0620(16) Uani d . 1 . . C
H12 -.3925 -.2372 -.3250 .074 Uiso calc R 1 . . H
C13 -.2737(5) -.2192(7) -.1825(4) .0541(15) Uani d . 1 . . C
H13 -.2145 -.2620 -.2078 .065 Uiso calc R 1 . . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni .3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P .1023 .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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
P Ni P . 2 87.18(7)
P Ni Cl . 2 173.87(6)
P Ni Cl 2 2 87.78(4)
P Ni Cl . . 87.78(4)
P Ni Cl 2 . 173.87(6)
Cl Ni Cl 2 . 97.45(7)
C2 P C8 . . 108.1(2)
C2 P C1 . . 105.9(2)
C8 P C1 . . 106.0(2)
C2 P Ni . . 111.42(17)
C8 P Ni . . 116.05(15)
C1 P Ni . . 108.77(16)
C1 C1 P 2 . 109.9(3)
C1 C1 H1A 2 . 109.7
P C1 H1A . . 109.7
C1 C1 H1B 2 . 109.7
P C1 H1B . . 109.7
H1A C1 H1B . . 108.2
C7 C2 C3 . . 118.1(4)
C7 C2 P . . 122.6(4)
C3 C2 P . . 119.3(3)
C4 C3 C2 . . 120.7(4)
C4 C3 H3 . . 119.6
C2 C3 H3 . . 119.6
C5 C4 C3 . . 120.5(5)
C5 C4 H4 . . 119.7
C3 C4 H4 . . 119.7
C4 C5 C6 . . 119.5(5)
C4 C5 H5 . . 120.3
C6 C5 H5 . . 120.3
C5 C6 C7 . . 120.5(5)
C5 C6 H6 . . 119.7
C7 C6 H6 . . 119.7
C2 C7 C6 . . 120.6(5)
C2 C7 H7 . . 119.7
C6 C7 H7 . . 119.7
C9 C8 C13 . . 118.2(5)
C9 C8 P . . 121.4(4)
C13 C8 P . . 120.2(4)
C8 C9 C10 . . 120.8(5)
C8 C9 H9 . . 119.6
C10 C9 H9 . . 119.6
C11 C10 C9 . . 119.7(6)
C11 C10 H10 . . 120.2
C9 C10 H10 . . 120.2
C12 C11 C10 . . 119.9(5)
C12 C11 H11 . . 120.0
C10 C11 H11 . . 120.0
C11 C12 C13 . . 120.2(5)
C11 C12 H12 . . 119.9
C13 C12 H12 . . 119.9
C8 C13 C12 . . 121.1(5)
C8 C13 H13 . . 119.4
C12 C13 H13 . . 119.4
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni P . 2.1346(13) ?
Ni P 2 2.1346(13) ?
Ni Cl 2 2.2054(13) ?
Ni Cl . 2.2054(13) ?
P C2 . 1.800(4) ?
P C8 . 1.804(5) ?
P C1 . 1.836(4) ?
C1 C1 2 1.413(10) ?
C1 H1A . .9900 ?
C1 H1B . .9900 ?
C2 C7 . 1.383(6) ?
C2 C3 . 1.392(6) ?
C3 C4 . 1.381(7) ?
C3 H3 . .9500 ?
C4 C5 . 1.366(7) ?
C4 H4 . .9500 ?
C5 C6 . 1.373(7) ?
C5 H5 . .9500 ?
C6 C7 . 1.384(7) ?
C6 H6 . .9500 ?
C7 H7 . .9500 ?
C8 C9 . 1.364(7) ?
C8 C13 . 1.384(7) ?
C9 C10 . 1.407(8) ?
C9 H9 . .9500 ?
C10 C11 . 1.376(7) ?
C10 H10 . .9500 ?
C11 C12 . 1.354(8) ?
C11 H11 . .9500 ?
C12 C13 . 1.388(8) ?
C12 H12 . .9500 ?
C13 H13 . .9500 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C1 H1A Cl 1_545 .99 2.69 3.556(4) 147
C12 H12 Cl 4_444 .95 2.74 3.664(6) 166
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
P Ni P C2 2 . . 106.36(17)
Cl Ni P C2 . . . -70.14(15)
P Ni P C8 2 . . -129.38(19)
Cl Ni P C8 . . . 54.11(17)
P Ni P C1 2 . . -10.0(2)
Cl Ni P C1 . . . 173.5(2)
C2 P C1 C1 . . 2 -85.2(5)
C8 P C1 C1 . . 2 160.1(5)
Ni P C1 C1 . . 2 34.6(5)
C8 P C2 C7 . . . 43.2(4)
C1 P C2 C7 . . . -70.0(4)
Ni P C2 C7 . . . 171.9(3)
C8 P C2 C3 . . . -137.6(4)
C1 P C2 C3 . . . 109.1(4)
Ni P C2 C3 . . . -9.0(4)
C7 C2 C3 C4 . . . -2.0(7)
P C2 C3 C4 . . . 178.8(4)
C2 C3 C4 C5 . . . .3(7)
C3 C4 C5 C6 . . . 1.0(8)
C4 C5 C6 C7 . . . -.5(8)
C3 C2 C7 C6 . . . 2.6(7)
P C2 C7 C6 . . . -178.3(4)
C5 C6 C7 C2 . . . -1.4(7)
C2 P C8 C9 . . . 28.5(5)
C1 P C8 C9 . . . 141.7(4)
Ni P C8 C9 . . . -97.4(4)
C2 P C8 C13 . . . -156.2(4)
C1 P C8 C13 . . . -43.0(4)
Ni P C8 C13 . . . 77.8(4)
C13 C8 C9 C10 . . . 1.8(8)
P C8 C9 C10 . . . 177.2(4)
C8 C9 C10 C11 . . . -.1(9)
C9 C10 C11 C12 . . . -.7(9)
C10 C11 C12 C13 . . . -.1(9)
C9 C8 C13 C12 . . . -2.7(8)
P C8 C13 C12 . . . -178.1(4)
C11 C12 C13 C8 . . . 1.9(8)
P C1 C1 P . 2 2 -42.7(6)
