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#$Date: 2016-03-21 19:15:46 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178842 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/96/4109676.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_4109676
loop_
_publ_author_name
'Dieter Meinhard'
'Marcus Wegner'
'Georgy Kipiani'
'Andrew Hearley'
'Peter Reuter'
'Stefan Fischer'
'Othmar Marti'
'Bernhard Rieger'
_publ_contact_author_address
;Albert-Einstein Allee 11
D-89081 Ulm
Germany
;
_publ_contact_author_email       bernhard.rieger@uni-ulm.de
_publ_contact_author_fax         '+49 731 502 303 9'
_publ_contact_author_name        'Prof. Dr. Bernhard Rieger'
_publ_contact_author_phone       '+49 731 502 303 8'
_publ_section_title
;
 New Nickel(II) Diimine Complexes and the Control of Polyethylene
 Microstructure by Catalyst Design
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9182
_journal_page_last               9191
_journal_paper_doi               10.1021/ja070224i
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C47 H43 N2 Ni O2, Cl6 Sb'
_chemical_formula_sum            'C47 H43 Cl6 N2 Ni O2 Sb'
_chemical_formula_weight         1060.99
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 113.106(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.4769(19)
_cell_length_b                   17.0447(18)
_cell_length_c                   17.628(2)
_cell_measurement_reflns_used    4399
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.94
_cell_measurement_theta_min      2.39
_cell_volume                     4829.9(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Stoe IPDS diffractometer'
_diffrn_measurement_method       'φ rotation 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  0.0689
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18762
_diffrn_reflns_theta_full        25.94
_diffrn_reflns_theta_max         25.94
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count image
_diffrn_standards_interval_time  4.50
_diffrn_standards_number         '50 to 200'
_exptl_absorpt_coefficient_mu    1.319
_exptl_absorpt_correction_T_max  0.8947
_exptl_absorpt_correction_T_min  0.6740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing (1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       plate
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.886
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4399
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0835P)²+0.4847P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1481
_reflns_number_gt                2963
_reflns_number_total             4399
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja070224isi20070131_031055.cif
_cod_data_source_block           kip487a
_cod_original_cell_volume        4829.9(9)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4109676
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'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
C1 C 0.3040(3) 0.3191(2) 0.4728(3) 0.0536(11) Uani 1 1 d .
C2 C 0.2500 0.3572(4) 0.5000 0.063(2) Uani 1 2 d S
C3 C 0.3640(4) 0.3647(3) 0.4484(4) 0.0805(18) Uani 1 1 d .
H3A H 0.3966 0.3292 0.4312 0.121 Uiso 1 1 calc R
H3B H 0.3999 0.3949 0.4946 0.121 Uiso 1 1 calc R
H3C H 0.3337 0.3994 0.4037 0.121 Uiso 1 1 calc R
C4 C 0.2760(3) 0.0195(2) 0.4759(3) 0.0445(10) Uani 1 1 d .
C5 C 0.3017(4) -0.0554(3) 0.4490(3) 0.0624(14) Uani 1 1 d .
H5A H 0.3349 -0.0441 0.4180 0.094 Uiso 1 1 calc R
H5B H 0.2531 -0.0843 0.4150 0.094 Uiso 1 1 calc R
H5C H 0.3336 -0.0862 0.4966 0.094 Uiso 1 1 calc R
C6 C 0.3407(3) 0.1025(2) 0.4070(3) 0.0466(11) Uani 1 1 d .
C7 C 0.2975(3) 0.0974(2) 0.3215(3) 0.0525(11) Uani 1 1 d .
C8 C 0.3384(4) 0.1177(3) 0.2706(3) 0.0594(13) Uani 1 1 d .
H8 H 0.3102 0.1136 0.2137 0.071 Uiso 1 1 calc R
C9 C 0.4200(4) 0.1438(3) 0.3023(3) 0.0600(13) Uani 1 1 d .
C10 C 0.4626(5) 0.1657(4) 0.2453(4) 0.0840(18) Uani 1 1 d .
H10A H 0.5180 0.1837 0.2774 0.126 Uiso 1 1 calc R
H10B H 0.4317 0.2067 0.2087 0.126 Uiso 1 1 calc R
H10C H 0.4650 0.1207 0.2137 0.126 Uiso 1 1 calc R
C11 C 0.4606(3) 0.1479(3) 0.3870(3) 0.0567(12) Uani 1 1 d .
H11 H 0.5156 0.1650 0.4091 0.068 Uiso 1 1 calc R
C12 C 0.4233(3) 0.1277(2) 0.4411(3) 0.0478(10) Uani 1 1 d .
C13 C 0.4747(3) 0.1317(3) 0.5307(3) 0.0524(11) Uani 1 1 d .
C14 C 0.4882(3) 0.0666(3) 0.5822(3) 0.0583(12) Uani 1 1 d .
H14 H 0.4587 0.0205 0.5618 0.070 Uiso 1 1 calc R
C15 C 0.5446(4) 0.0697(3) 0.6630(4) 0.0734(16) Uani 1 1 d .
H15 H 0.5530 0.0258 0.6966 0.088 Uiso 1 1 calc R
C16 C 0.5885(4) 0.1373(4) 0.6942(4) 0.0820(18) Uani 1 1 d .
H16 H 0.6274 0.1388 0.7484 0.098 Uiso 1 1 calc R
C17 C 0.5747(4) 0.2027(4) 0.6450(4) 0.0797(17) Uani 1 1 d .
H17 H 0.6033 0.2489 0.6665 0.096 Uiso 1 1 calc R
C18 C 0.5193(4) 0.2002(3) 0.5648(4) 0.0735(16) Uani 1 1 d .
H18 H 0.5110 0.2448 0.5321 0.088 Uiso 1 1 calc R
C19 C 0.2086(3) 0.0727(3) 0.2800(3) 0.0560(12) Uani 1 1 d .
C20 C 0.1881(4) 0.0003(4) 0.2416(4) 0.0769(16) Uani 1 1 d .
H20 H 0.2301 -0.0358 0.2477 0.092 Uiso 1 1 calc R
C21 C 0.1068(5) -0.0191(5) 0.1945(4) 0.096(2) Uani 1 1 d .
H21 H 0.0939 -0.0680 0.1695 0.115 Uiso 1 1 calc R
C22 C 0.0447(5) 0.0342(6) 0.1846(5) 0.100(2) Uani 1 1 d .
H22 H -0.0103 0.0215 0.1522 0.120 Uiso 1 1 calc R
C23 C 0.0631(5) 0.1051(5) 0.2220(5) 0.094(2) Uani 1 1 d .
H23 H 0.0207 0.1409 0.2150 0.113 Uiso 1 1 calc R
C24 C 0.1448(4) 0.1247(4) 0.2706(4) 0.0772(16) Uani 1 1 d .
H24 H 0.1568 0.1731 0.2970 0.093 Uiso 1 1 calc R
N1 N 0.2958(2) 0.08925(18) 0.4599(2) 0.0425(8) Uani 1 1 d .
Ni1 Ni 0.2500 0.17265(4) 0.5000 0.0415(2) Uani 1 2 d S
O1 O 0.3072(2) 0.24428(17) 0.4664(2) 0.0552(8) Uani 1 1 d .
Cl1 Cl 0.2012(3) 0.74500(12) 0.39881(18) 0.268(3) Uani 1 1 d .
Cl2 Cl 0.3801(2) 0.6418(3) 0.4912(3) 0.245(3) Uani 1 1 d .
Cl3 Cl 0.20162(12) 0.55016(9) 0.39727(9) 0.0923(5) Uani 1 1 d .
Sb1 Sb 0.2500 0.64806(3) 0.5000 0.0769(2) Uani 1 2 d S
H4 H 0.2500 0.411(5) 0.5000 0.09(3) Uiso 1 2 d S
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'
N N 0.0061 0.0033 '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'
O O 0.0106 0.0060 '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'
Sb Sb -0.5866 1.5461 '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
O1 C1 C2 124.0(4) . .
O1 C1 C3 115.5(4) . .
C2 C1 C3 120.5(4) . .
C1 C2 C1 123.8(6) . 2_556
N1 C4 C4 113.8(2) . 2_556
N1 C4 C5 125.1(4) . .
C4 C4 C5 121.1(2) 2_556 .
C12 C6 C7 120.9(4) . .
C12 C6 N1 120.0(4) . .
C7 C6 N1 118.8(4) . .
C8 C7 C6 118.7(5) . .
C8 C7 C19 116.9(4) . .
C6 C7 C19 124.3(4) . .
C9 C8 C7 121.9(5) . .
C11 C9 C8 117.6(4) . .
C11 C9 C10 121.8(5) . .
C8 C9 C10 120.6(5) . .
C9 C11 C12 123.2(5) . .
C11 C12 C6 117.7(4) . .
C11 C12 C13 117.8(4) . .
C6 C12 C13 124.5(4) . .
C14 C13 C18 117.4(5) . .
C14 C13 C12 122.3(4) . .
C18 C13 C12 119.9(4) . .
C15 C14 C13 120.7(5) . .
C16 C15 C14 120.5(5) . .
C17 C16 C15 119.7(6) . .
C18 C17 C16 120.4(6) . .
C17 C18 C13 121.3(5) . .
C24 C19 C20 118.2(6) . .
C24 C19 C7 120.8(5) . .
C20 C19 C7 120.6(5) . .
C21 C20 C19 121.0(6) . .
C20 C21 C22 119.8(7) . .
C23 C22 C21 120.2(7) . .
C22 C23 C24 120.4(7) . .
C19 C24 C23 120.4(6) . .
C4 N1 C6 122.6(3) . .
C4 N1 Ni1 114.6(3) . .
C6 N1 Ni1 122.4(2) . .
O1 Ni1 O1 95.67(19) . 2_556
O1 Ni1 N1 171.89(15) . 2_556
O1 Ni1 N1 90.86(14) 2_556 2_556
O1 Ni1 N1 90.86(14) . .
O1 Ni1 N1 171.89(15) 2_556 .
N1 Ni1 N1 83.1(2) 2_556 .
C1 O1 Ni1 126.1(3) . .
Cl1 Sb1 Cl1 89.84(13) 2_556 .
Cl1 Sb1 Cl2 90.6(2) 2_556 .
Cl1 Sb1 Cl2 93.12(17) . .
Cl1 Sb1 Cl2 93.12(17) 2_556 2_556
Cl1 Sb1 Cl2 90.6(2) . 2_556
Cl2 Sb1 Cl2 174.8(3) . 2_556
Cl1 Sb1 Cl3 179.50(15) 2_556 .
Cl1 Sb1 Cl3 90.04(8) . .
Cl2 Sb1 Cl3 88.94(14) . .
Cl2 Sb1 Cl3 87.36(11) 2_556 .
Cl1 Sb1 Cl3 90.04(8) 2_556 2_556
Cl1 Sb1 Cl3 179.50(15) . 2_556
Cl2 Sb1 Cl3 87.36(11) . 2_556
Cl2 Sb1 Cl3 88.94(14) 2_556 2_556
Cl3 Sb1 Cl3 90.08(7) . 2_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.284(5) .
C1 C2 1.378(6) .
C1 C3 1.497(7) .
C2 C1 1.378(6) 2_556
C4 N1 1.299(5) .
C4 C4 1.469(8) 2_556
C4 C5 1.492(6) .
C6 C12 1.394(7) .
C6 C7 1.399(7) .
C6 N1 1.453(5) .
C7 C8 1.394(7) .
C7 C19 1.495(7) .
C8 C9 1.385(8) .
C9 C11 1.381(8) .
C9 C10 1.512(7) .
C11 C12 1.394(6) .
C12 C13 1.481(7) .
C13 C14 1.394(7) .
C13 C18 1.400(7) .
C14 C15 1.380(8) .
C15 C16 1.374(9) .
C16 C17 1.374(9) .
C17 C18 1.366(8) .
C19 C24 1.381(8) .
C19 C20 1.386(7) .
C20 C21 1.376(9) .
C21 C22 1.373(11) .
C22 C23 1.353(11) .
C23 C24 1.388(10) .
N1 Ni1 1.899(3) .
Ni1 O1 1.819(3) .
Ni1 O1 1.819(3) 2_556
Ni1 N1 1.899(3) 2_556
Cl1 Sb1 2.334(2) .
Cl2 Sb1 2.343(4) .
Cl3 Sb1 2.3615(15) .
Sb1 Cl1 2.334(2) 2_556
Sb1 Cl2 2.343(4) 2_556
Sb1 Cl3 2.3615(15) 2_556
