#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/92/2019290.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_2019290
loop_
_publ_author_name
'Schultz, Madeleine'
'Plessow, Philipp-Nikolaus'
'Rominger, Frank'
'Weigel, Laura'
_publ_section_title
;
 Structure, magnetism and colour in simple bis(phosphine)nickel(II)
 dihalide complexes: an experimental and theoretical investigation
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1437
_journal_page_last               1447
_journal_paper_doi               10.1107/S0108270113030692
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Ni I2 (C26 H24 P2)], C H2 Cl2'
_chemical_formula_moiety         'C26 H24 I2 Ni P2, C H2 Cl2'
_chemical_formula_sum            'C27 H26 Cl2 I2 Ni P2'
_chemical_formula_weight         795.83
_chemical_name_systematic
;[1,2-Bis(diphenylphosphanyl)ethane-κ²P,P']diiodidonickel(II)
dichloromethane monosolvate
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_Hall           'I 4bw -2c'
_space_group_name_H-M_alt        'I 41 c d'
_symmetry_space_group_name_Hall  'I 4bw -2c'
_symmetry_space_group_name_H-M   'I 41 c d'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   26.3705(17)
_cell_length_b                   26.3705(17)
_cell_length_c                   16.7900(11)
_cell_measurement_reflns_used    9238
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.80
_cell_measurement_theta_min      2.44
_cell_volume                     11675.8(13)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008b)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008b)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008b)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008b)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            109821
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.129
_diffrn_reflns_theta_min         1.544
_exptl_absorpt_coefficient_mu    3.088
_exptl_absorpt_correction_T_max  0.8497
_exptl_absorpt_correction_T_min  0.6521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2008a)
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             6176
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.318
_refine_diff_density_min         -1.258
_refine_ls_abs_structure_details
;
Flack x determined using 3206 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons & Flack, 2004)
;
_refine_ls_abs_structure_Flack   -0.004(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         7839
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0204P)²+71.4066P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0746
_reflns_number_gt                7131
_reflns_number_total             7839
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fa3325.cif
_cod_data_source_block           lw29
_cod_original_cell_volume        11675.8(17)
_cod_database_code               2019290
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.429
_shelx_estimated_absorpt_t_max   0.861
_shelxl_version_number           2.013
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-y, x+1/2, z+1/4'
'y+1/2, -x, z+3/4'
'x, -y, z+1/2'
'-x+1/2, y+1/2, z'
'-y, -x+1/2, z+3/4'
'y+1/2, x, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1, z+1'
'-y+1/2, x+1, z+3/4'
'y+1, -x+1/2, z+5/4'
'x+1/2, -y+1/2, z+1'
'-x+1, y+1, z+1/2'
'-y+1/2, -x+1, z+5/4'
'y+1, x+1/2, z+3/4'
loop_
_atom_site_type_symbol
_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_occupancy
Ni Ni1 0.28453(3) 1.00312(3) 0.32327(5) 0.02110(15) Uani d 1
I I1 0.23025(2) 1.05229(2) 0.42006(3) 0.03191(10) Uani d 1
I I2 0.34232(2) 0.96692(2) 0.42855(3) 0.03574(11) Uani d 1
P P1 0.33005(6) 0.96805(6) 0.23176(10) 0.0209(3) Uani d 1
P P2 0.23797(6) 1.03270(6) 0.22710(10) 0.0222(3) Uani d 1
C C9 0.2906(3) 0.9621(3) 0.1424(4) 0.0273(14) Uani d 1
H H9A 0.3120 0.9539 0.0956 0.033 Uiso calc 1
H H9B 0.2655 0.9346 0.1495 0.033 Uiso calc 1
C C10 0.2640(3) 1.0122(3) 0.1299(4) 0.0275(14) Uani d 1
H H10A 0.2363 1.0083 0.0906 0.033 Uiso calc 1
H H10B 0.2883 1.0378 0.1096 0.033 Uiso calc 1
C C11 0.3575(3) 0.9055(2) 0.2422(4) 0.0257(13) Uani d 1
C C12 0.4077(3) 0.8949(3) 0.2251(4) 0.0330(15) Uani d 1
H H12 0.4303 0.9217 0.2121 0.040 Uiso calc 1
C C13 0.4251(3) 0.8453(3) 0.2269(5) 0.0416(19) Uani d 1
H H13 0.4594 0.8381 0.2136 0.050 Uiso calc 1
C C14 0.3932(4) 0.8066(3) 0.2478(5) 0.046(2) Uani d 1
H H14 0.4054 0.7727 0.2490 0.055 Uiso calc 1
C C15 0.3430(4) 0.8166(3) 0.2671(6) 0.052(2) Uani d 1
H H15 0.3208 0.7899 0.2819 0.062 Uiso calc 1
C C16 0.3259(3) 0.8658(3) 0.2645(5) 0.0411(18) Uani d 1
H H16 0.2917 0.8729 0.2782 0.049 Uiso calc 1
C C21 0.3806(2) 1.0109(2) 0.2024(4) 0.0246(13) Uani d 1
C C22 0.3958(3) 1.0497(3) 0.2528(4) 0.0345(16) Uani d 1
H H22 0.3814 1.0526 0.3044 0.041 Uiso calc 1
C C23 0.4322(3) 1.0845(3) 0.2280(5) 0.044(2) Uani d 1
H H23 0.4423 1.1113 0.2623 0.053 Uiso calc 1
C C24 0.4539(3) 1.0798(3) 0.1525(5) 0.045(2) Uani d 1
H H24 0.4791 1.1032 0.1355 0.053 Uiso calc 1
C C25 0.4389(3) 1.0419(3) 0.1034(5) 0.0423(19) Uani d 1
H H25 0.4536 1.0391 0.0519 0.051 Uiso calc 1
C C26 0.4023(3) 1.0069(3) 0.1275(4) 0.0331(16) Uani d 1
H H26 0.3923 0.9804 0.0926 0.040 Uiso calc 1
C C31 0.1743(3) 1.0062(3) 0.2245(4) 0.0269(13) Uani d 1
C C32 0.1382(3) 1.0263(3) 0.1712(5) 0.0359(15) Uani d 1
H H32 0.1459 1.0556 0.1406 0.043 Uiso calc 1
C C33 0.0915(3) 1.0027(4) 0.1641(5) 0.0436(18) Uani d 1
H H33 0.0668 1.0164 0.1289 0.052 Uiso calc 1
C C34 0.0803(3) 0.9597(3) 0.2074(5) 0.045(2) Uani d 1
H H34 0.0485 0.9433 0.2012 0.054 Uiso calc 1
C C35 0.1161(3) 0.9407(3) 0.2600(5) 0.0414(19) Uani d 1
H H35 0.1084 0.9116 0.2910 0.050 Uiso calc 1
C C36 0.1624(3) 0.9638(3) 0.2676(5) 0.0323(15) Uani d 1
H H36 0.1867 0.9501 0.3034 0.039 Uiso calc 1
C C41 0.2344(3) 1.1014(3) 0.2191(4) 0.0274(14) Uani d 1
C C42 0.1910(3) 1.1283(3) 0.2384(5) 0.0339(16) Uani d 1
H H42 0.1614 1.1116 0.2569 0.041 Uiso calc 1
C C43 0.1923(4) 1.1809(3) 0.2297(6) 0.051(2) Uani d 1
H H43 0.1626 1.2000 0.2408 0.061 Uiso calc 1
C C44 0.2351(4) 1.2059(3) 0.2057(6) 0.053(2) Uani d 1
H H44 0.2349 1.2418 0.2010 0.064 Uiso calc 1
C C45 0.2784(4) 1.1790(3) 0.1885(6) 0.048(2) Uani d 1
H H45 0.3082 1.1962 0.1717 0.058 Uiso calc 1
C C46 0.2782(3) 1.1266(3) 0.1957(5) 0.0362(17) Uani d 1
H H46 0.3081 1.1078 0.1846 0.043 Uiso calc 1
C C51 0.1612(7) 0.8227(5) 0.1681(10) 0.154(7) Uani d 1
H H51A 0.1651 0.7885 0.1445 0.184 Uiso calc 1
H H51B 0.1246 0.8309 0.1680 0.184 Uiso calc 1
Cl Cl1 0.1907(2) 0.8642(2) 0.1089(3) 0.167(3) Uani d 1
Cl Cl2 0.18145(19) 0.81989(16) 0.2668(4) 0.144(2) Uani d 1
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'
Cl Cl 0.1484 0.1585 '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'
I I -0.4742 1.8119 '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
P1 Ni1 P2 86.51(7)
P1 Ni1 I2 90.04(5)
P2 Ni1 I2 176.51(6)
P1 Ni1 I1 173.72(6)
P2 Ni1 I1 88.49(5)
I2 Ni1 I1 94.93(3)
C11 P1 C21 107.5(3)
C11 P1 C9 103.1(3)
C21 P1 C9 104.3(3)
C11 P1 Ni1 123.0(2)
C21 P1 Ni1 109.6(2)
C9 P1 Ni1 107.7(2)
C41 P2 C31 109.4(3)
C41 P2 C10 104.2(3)
C31 P2 C10 102.1(3)
C41 P2 Ni1 116.2(2)
C31 P2 Ni1 113.7(2)
C10 P2 Ni1 109.9(2)
C10 C9 P1 107.5(4)
C10 C9 H9A 110.2
P1 C9 H9A 110.2
C10 C9 H9B 110.2
P1 C9 H9B 110.2
H9A C9 H9B 108.5
C9 C10 P2 107.8(4)
C9 C10 H10A 110.1
P2 C10 H10A 110.1
C9 C10 H10B 110.1
P2 C10 H10B 110.1
H10A C10 H10B 108.5
C12 C11 C16 118.6(7)
C12 C11 P1 123.1(5)
C16 C11 P1 118.2(6)
C11 C12 C13 120.1(7)
C11 C12 H12 119.9
C13 C12 H12 119.9
C14 C13 C12 120.3(8)
C14 C13 H13 119.8
C12 C13 H13 119.8
C13 C14 C15 120.3(8)
C13 C14 H14 119.9
C15 C14 H14 119.9
C16 C15 C14 119.1(8)
C16 C15 H15 120.5
C14 C15 H15 120.5
C15 C16 C11 121.5(8)
C15 C16 H16 119.2
C11 C16 H16 119.2
C26 C21 C22 119.3(7)
C26 C21 P1 120.2(5)
C22 C21 P1 120.4(5)
C21 C22 C23 120.3(7)
C21 C22 H22 119.9
C23 C22 H22 119.9
C22 C23 C24 119.7(8)
C22 C23 H23 120.1
C24 C23 H23 120.1
C25 C24 C23 119.9(8)
C25 C24 H24 120.0
C23 C24 H24 120.0
C24 C25 C26 120.9(8)
C24 C25 H25 119.6
C26 C25 H25 119.6
C21 C26 C25 120.0(7)
C21 C26 H26 120.0
C25 C26 H26 120.0
C36 C31 C32 119.3(7)
C36 C31 P2 120.8(6)
C32 C31 P2 119.6(5)
C33 C32 C31 119.1(8)
C33 C32 H32 120.4
C31 C32 H32 120.4
C34 C33 C32 120.9(8)
C34 C33 H33 119.5
C32 C33 H33 119.5
C33 C34 C35 119.1(7)
C33 C34 H34 120.4
C35 C34 H34 120.4
C36 C35 C34 120.4(8)
C36 C35 H35 119.8
C34 C35 H35 119.8
C31 C36 C35 121.1(7)
C31 C36 H36 119.4
C35 C36 H36 119.4
C42 C41 C46 120.4(7)
C42 C41 P2 122.5(6)
C46 C41 P2 117.0(5)
C41 C42 C43 117.8(8)
C41 C42 H42 121.1
C43 C42 H42 121.1
C44 C43 C42 122.0(9)
C44 C43 H43 119.0
C42 C43 H43 119.0
C43 C44 C45 119.9(8)
C43 C44 H44 120.0
C45 C44 H44 120.0
C44 C45 C46 119.4(8)
C44 C45 H45 120.3
C46 C45 H45 120.3
C45 C46 C41 120.3(8)
C45 C46 H46 119.8
C41 C46 H46 119.8
Cl1 C51 Cl2 116.9(9)
Cl1 C51 H51A 108.1
Cl2 C51 H51A 108.1
Cl1 C51 H51B 108.1
Cl2 C51 H51B 108.1
H51A C51 H51B 107.3
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ni1 P1 2.1582(18)
Ni1 P2 2.1733(18)
Ni1 I2 2.5216(9)
Ni1 I1 2.5240(9)
P1 C11 1.811(7)
P1 C21 1.816(7)
P1 C9 1.832(7)
P2 C41 1.818(7)
P2 C31 1.820(7)
P2 C10 1.851(6)
C9 C10 1.512(9)
C9 H9A 0.9900
C9 H9B 0.9900
C10 H10A 0.9900
C10 H10B 0.9900
C11 C12 1.383(10)
C11 C16 1.387(10)
C12 C13 1.388(10)
C12 H12 0.9500
C13 C14 1.370(12)
C13 H13 0.9500
C14 C15 1.387(13)
C14 H14 0.9500
C15 C16 1.375(11)
C15 H15 0.9500
C16 H16 0.9500
C21 C26 1.385(9)
C21 C22 1.388(10)
C22 C23 1.390(10)
C22 H22 0.9500
C23 C24 1.397(12)
C23 H23 0.9500
C24 C25 1.353(12)
C24 H24 0.9500
C25 C26 1.395(10)
C25 H25 0.9500
C26 H26 0.9500
C31 C36 1.368(10)
C31 C32 1.408(10)
C32 C33 1.385(10)
C32 H32 0.9500
C33 C34 1.379(13)
C33 H33 0.9500
C34 C35 1.385(13)
C34 H34 0.9500
C35 C36 1.372(10)
C35 H35 0.9500
C36 H36 0.9500
C41 C42 1.385(10)
C41 C46 1.389(10)
C42 C43 1.394(11)
C42 H42 0.9500
C43 C44 1.365(13)
C43 H43 0.9500
C44 C45 1.375(13)
C44 H44 0.9500
C45 C46 1.387(11)
C45 H45 0.9500
C46 H46 0.9500
C51 Cl1 1.670(14)
C51 Cl2 1.743(15)
C51 H51A 0.9900
C51 H51B 0.9900
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
C11 P1 C9 C10 177.8(5)
C21 P1 C9 C10 -70.0(5)
Ni1 P1 C9 C10 46.4(5)
P1 C9 C10 P2 -46.2(5)
C41 P2 C10 C9 154.2(5)
C31 P2 C10 C9 -92.0(5)
Ni1 P2 C10 C9 29.0(5)
C21 P1 C11 C12 -3.4(7)
C9 P1 C11 C12 106.5(6)
Ni1 P1 C11 C12 -131.9(5)
C21 P1 C11 C16 -180.0(6)
C9 P1 C11 C16 -70.1(6)
Ni1 P1 C11 C16 51.5(7)
C16 C11 C12 C13 2.9(11)
P1 C11 C12 C13 -173.7(6)
C11 C12 C13 C14 -1.8(13)
C12 C13 C14 C15 0.2(13)
C13 C14 C15 C16 0.4(14)
C14 C15 C16 C11 0.7(14)
C12 C11 C16 C15 -2.3(13)
P1 C11 C16 C15 174.4(7)
C11 P1 C21 C26 68.9(6)
C9 P1 C21 C26 -40.2(6)
Ni1 P1 C21 C26 -155.3(5)
C11 P1 C21 C22 -114.9(6)
C9 P1 C21 C22 136.0(6)
Ni1 P1 C21 C22 20.9(6)
C26 C21 C22 C23 0.5(12)
P1 C21 C22 C23 -175.8(6)
C21 C22 C23 C24 -0.8(13)
C22 C23 C24 C25 0.8(14)
C23 C24 C25 C26 -0.6(14)
C22 C21 C26 C25 -0.2(11)
P1 C21 C26 C25 176.0(6)
C24 C25 C26 C21 0.3(13)
C41 P2 C31 C36 -146.0(6)
C10 P2 C31 C36 104.1(6)
Ni1 P2 C31 C36 -14.2(6)
C41 P2 C31 C32 40.9(7)
C10 P2 C31 C32 -69.1(6)
Ni1 P2 C31 C32 172.6(5)
C36 C31 C32 C33 0.4(11)
P2 C31 C32 C33 173.7(6)
C31 C32 C33 C34 -1.0(12)
C32 C33 C34 C35 1.5(13)
C33 C34 C35 C36 -1.4(12)
C32 C31 C36 C35 -0.3(11)
P2 C31 C36 C35 -173.5(6)
C34 C35 C36 C31 0.8(12)
C31 P2 C41 C42 22.0(7)
C10 P2 C41 C42 130.5(6)
Ni1 P2 C41 C42 -108.4(6)
C31 P2 C41 C46 -160.8(5)
C10 P2 C41 C46 -52.3(6)
Ni1 P2 C41 C46 68.8(6)
C46 C41 C42 C43 3.1(11)
P2 C41 C42 C43 -179.7(6)
C41 C42 C43 C44 -2.3(14)
C42 C43 C44 C45 0.8(16)
C43 C44 C45 C46 -0.1(15)
C44 C45 C46 C41 0.9(13)
C42 C41 C46 C45 -2.5(11)
P2 C41 C46 C45 -179.8(6)
