#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:49:05 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179156 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/17/4311717.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_4311717
loop_
_publ_author_name
'Shane G. Telfer'
'Tomohiro Sato'
'Takunori Harada'
'Reiko Kuroda'
'Julie Lefebvre'
'Daniel B. Leznoff'
_publ_section_title
;
 Mono- and Dinuclear Complexes of Chiral Tri- and Tetradentate Schiff-Base
 Ligands Derived from 1,1'-Binaphthyl-2,2'-diamine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6168
_journal_page_last               6176
_journal_paper_doi               10.1021/ic049910y
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C53.5 H43 Cl2 N7 Ni O10.5'
_chemical_formula_weight         1081.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           154
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   11.6939(4)
_cell_length_b                   11.6939(4)
_cell_length_c                   33.013(2)
_cell_measurement_reflns_used    5110
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      1.85
_cell_volume                     3909.6(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_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  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            24426
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.550
_exptl_absorpt_correction_T_max  0.9730
_exptl_absorpt_correction_T_min  0.7705
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1803
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.174
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         6148
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0734
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1423P)²+4.1540P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2043
_refine_ls_wR_factor_ref         0.2130
_reflns_number_gt                5110
_reflns_number_total             6148
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049910ysi20040122_090530_1.cif
_cod_data_source_block           Fig1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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_cell_volume        3909.7(3)
_cod_original_sg_symbol_H-M      'P 31 2 1'
_cod_database_code               4311717
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'x-y, -y, -z+1/3'
'-x, -x+y, -z+2/3'
'y, x, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2807(5) 0.0435(5) 0.92507(12) 0.0195(9) Uani 1 1 d . . .
C2 C 0.1815(4) 0.0724(5) 0.91425(13) 0.0197(9) Uani 1 1 d . . .
C3 C 0.1980(5) 0.1553(6) 0.88116(15) 0.0289(11) Uani 1 1 d . . .
H3 H 0.1332 0.1768 0.8754 0.035 Uiso 1 1 calc R . .
C4 C 0.3071(5) 0.2040(6) 0.85759(14) 0.0320(12) Uani 1 1 d . . .
H4 H 0.3150 0.2567 0.8355 0.038 Uiso 1 1 calc R . .
C5 C 0.5211(5) 0.2201(6) 0.84053(16) 0.0379(14) Uani 1 1 d . . .
H5 H 0.5292 0.2702 0.8177 0.046 Uiso 1 1 calc R . .
C6 C 0.6162(5) 0.1908(6) 0.84863(15) 0.0347(12) Uani 1 1 d . . .
H6 H 0.6874 0.2186 0.8310 0.042 Uiso 1 1 calc R . .
C7 C 0.6088(5) 0.1178(5) 0.88373(14) 0.0273(11) Uani 1 1 d . . .
H7 H 0.6765 0.1006 0.8896 0.033 Uiso 1 1 calc R . .
C8 C 0.5018(5) 0.0725(5) 0.90909(13) 0.0240(10) Uani 1 1 d . . .
H8 H 0.4986 0.0260 0.9323 0.029 Uiso 1 1 calc R . .
C9 C 0.3962(5) 0.0954(5) 0.90050(13) 0.0235(10) Uani 1 1 d . . .
C10 C 0.4081(5) 0.1765(5) 0.86595(13) 0.0257(10) Uani 1 1 d . . .
C11 C 0.2666(4) -0.0436(5) 0.96009(12) 0.0191(9) Uani 1 1 d . . .
C12 C 0.2692(4) -0.0027(5) 0.99976(13) 0.0206(9) Uani 1 1 d . . .
C13 C 0.2716(5) -0.0773(5) 1.03291(14) 0.0246(10) Uani 1 1 d . . .
H13 H 0.2760 -0.0470 1.0592 0.030 Uiso 1 1 calc R . .
C14 C 0.2673(5) -0.1968(5) 1.02586(14) 0.0255(10) Uani 1 1 d . . .
H14 H 0.2717 -0.2448 1.0477 0.031 Uiso 1 1 calc R . .
C15 C 0.2457(5) -0.3703(5) 0.97845(17) 0.0298(11) Uani 1 1 d . . .
H15 H 0.2477 -0.4208 0.9999 0.036 Uiso 1 1 calc R . .
C16 C 0.2324(5) -0.4175(5) 0.93964(18) 0.0359(12) Uani 1 1 d . . .
H16 H 0.2261 -0.4989 0.9349 0.043 Uiso 1 1 calc R . .
C17 C 0.2286(5) -0.3432(5) 0.90743(17) 0.0344(12) Uani 1 1 d . . .
H17 H 0.2165 -0.3773 0.8813 0.041 Uiso 1 1 calc R . .
C18 C 0.2421(5) -0.2207(5) 0.91306(14) 0.0241(10) Uani 1 1 d . . .
H18 H 0.2411 -0.1725 0.8908 0.029 Uiso 1 1 calc R . .
C19 C 0.2575(5) -0.1666(5) 0.95282(13) 0.0212(9) Uani 1 1 d . . .
C20 C 0.2563(4) -0.2464(5) 0.98642(14) 0.0226(9) Uani 1 1 d . . .
N21 N 0.0654(4) 0.0237(4) 0.93840(11) 0.0186(7) Uani 1 1 d . . .
C22 C -0.0451(4) -0.0229(5) 0.92000(12) 0.0205(9) Uani 1 1 d . . .
H22 H -0.0488 -0.0336 0.8920 0.025 Uiso 1 1 calc R . .
C23 C -0.1643(4) -0.0589(5) 0.94260(13) 0.0214(8) Uani 1 1 d . . .
N24 N -0.1445(4) -0.0200(4) 0.98197(11) 0.0177(7) Uani 1 1 d . . .
C25 C -0.2514(5) -0.0500(5) 1.00490(14) 0.0236(10) Uani 1 1 d . . .
H25 H -0.2391 -0.0246 1.0320 0.028 Uiso 1 1 calc R . .
C26 C -0.3789(5) -0.1172(5) 0.98962(16) 0.0283(10) Uani 1 1 d . . .
H26 H -0.4503 -0.1359 1.0063 0.034 Uiso 1 1 calc R . .
C27 C -0.3990(5) -0.1553(6) 0.95049(16) 0.0348(13) Uani 1 1 d . . .
H27 H -0.4841 -0.2012 0.9400 0.042 Uiso 1 1 calc R . .
C28 C -0.2895(5) -0.1247(6) 0.92584(15) 0.0340(11) Uani 1 1 d . . .
H28 H -0.3009 -0.1483 0.8986 0.041 Uiso 1 1 calc R . .
N31 N 0.2585(4) 0.1106(4) 1.00730(11) 0.0214(8) Uani 1 1 d . . .
Ni Ni 0.05281(6) 0.05281(6) 1.0000 0.0157(2) Uani 1 2 d S . .
Cl1 Cl 0.5110(3) 0.4648(3) 0.95253(9) 0.0376(6) Uani 0.50 1 d P A 1
O11 O 0.3736(13) 0.3703(13) 0.9589(4) 0.056(3) Uiso 0.50 1 d P A 1
O12 O 0.5862(7) 0.3975(7) 0.94203(19) 0.0224(13) Uiso 0.50 1 d P A 1
O13 O 0.5613(11) 0.5516(11) 0.9851(3) 0.063(3) Uiso 0.50 1 d P A 1
O14 O 0.5208(7) 0.5389(7) 0.9166(2) 0.0278(15) Uiso 0.50 1 d P A 1
C91 C 0.4972(13) 0.4144(14) 0.9346(4) 0.041(3) Uiso 0.50 1 d P B 2
H91A H 0.5201 0.5055 0.9345 0.062 Uiso 0.50 1 calc PR B 2
H91B H 0.4967 0.3859 0.9073 0.062 Uiso 0.50 1 calc PR B 2
H91C H 0.5609 0.4043 0.9502 0.062 Uiso 0.50 1 calc PR B 2
O92 O 0.3832(11) 0.3446(11) 0.9501(3) 0.043(3) Uiso 0.50 1 d P B 2
Cl2 Cl 0.0000 0.29064(17) 0.8333 0.0385(5) Uani 1 2 d S . .
O21 O 0.0797(8) 0.3922(7) 0.8609(3) 0.145(5) Uani 1 1 d . . .
O22 O -0.0844(4) 0.1794(4) 0.85774(11) 0.0378(9) Uani 1 1 d . . .
N51 N 0.6188(11) -0.1522(11) 1.1245(3) 0.119(3) Uiso 1 1 d D . .
O52 O 0.7117(8) -0.1139(9) 1.0995(2) 0.103(2) Uiso 1 1 d D . .
O53 O 0.521(2) -0.128(3) 1.1171(7) 0.295(10) Uiso 1 1 d D . .
C54 C 0.5860(19) -0.2529(15) 1.1526(4) 0.149(6) Uiso 1 1 d D . .
H54A H 0.5444 -0.3366 1.1390 0.223 Uiso 1 1 calc R . .
H54B H 0.5264 -0.2514 1.1723 0.223 Uiso 1 1 calc R . .
H54C H 0.6646 -0.2398 1.1659 0.223 Uiso 1 1 calc R . .
H31A H 0.3011 0.1780 0.9871 0.050 Uiso 1 1 d . . .
H31B H 0.2714 0.1434 1.0318 0.050 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'
N N 0.0061 0.0033 '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'
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
_geom_angle_publ_flag
C2 C1 C9 118.3(4) . . ?
C2 C1 C11 122.5(4) . . ?
C9 C1 C11 119.2(4) . . ?
C1 C2 C3 121.1(4) . . ?
C1 C2 N21 119.8(4) . . ?
C3 C2 N21 119.0(4) . . ?
C4 C3 C2 120.8(5) . . ?
C3 C4 C10 121.1(4) . . ?
C6 C5 C10 121.9(5) . . ?
C5 C6 C7 120.5(5) . . ?
C8 C7 C6 120.1(5) . . ?
C7 C8 C9 121.2(4) . . ?
C8 C9 C1 122.4(4) . . ?
C8 C9 C10 118.3(4) . . ?
C1 C9 C10 119.2(4) . . ?
C4 C10 C5 122.7(5) . . ?
C4 C10 C9 119.5(4) . . ?
C5 C10 C9 117.8(5) . . ?
C12 C11 C19 119.3(4) . . ?
C12 C11 C1 121.2(4) . . ?
C19 C11 C1 119.4(4) . . ?
C11 C12 C13 121.6(5) . . ?
C11 C12 N31 119.4(4) . . ?
C13 C12 N31 118.8(4) . . ?
C14 C13 C12 119.3(4) . . ?
C13 C14 C20 121.2(4) . . ?
C16 C15 C20 121.3(5) . . ?
C15 C16 C17 119.7(5) . . ?
C18 C17 C16 121.8(5) . . ?
C17 C18 C19 120.6(5) . . ?
C11 C19 C18 122.5(4) . . ?
C11 C19 C20 120.0(4) . . ?
C18 C19 C20 117.4(4) . . ?
C14 C20 C15 122.5(4) . . ?
C14 C20 C19 118.4(4) . . ?
C15 C20 C19 119.1(4) . . ?
C22 N21 C2 117.6(4) . . ?
C22 N21 Ni 113.3(3) . . ?
C2 N21 Ni 127.8(3) . . ?
N21 C22 C23 120.1(4) . . ?
N24 C23 C28 121.7(4) . . ?
N24 C23 C22 114.7(4) . . ?
C28 C23 C22 123.6(4) . . ?
C25 N24 C23 118.0(4) . . ?
C25 N24 Ni 129.2(3) . . ?
C23 N24 Ni 112.0(3) . . ?
N24 C25 C26 122.5(4) . . ?
C27 C26 C25 119.7(5) . . ?
C26 C27 C28 119.0(5) . . ?
C23 C28 C27 119.1(5) . . ?
C12 N31 Ni 107.1(3) . . ?
N21 Ni N21 174.7(2) 6_557 . ?
N21 Ni N24 96.88(14) 6_557 . ?
N21 Ni N24 79.07(14) . . ?
N21 Ni N24 79.07(14) 6_557 6_557 ?
N21 Ni N24 96.88(14) . 6_557 ?
N24 Ni N24 82.86(19) . 6_557 ?
N21 Ni N31 90.08(14) 6_557 6_557 ?
N21 Ni N31 93.72(14) . 6_557 ?
N24 Ni N31 95.07(14) . 6_557 ?
N24 Ni N31 168.59(14) 6_557 6_557 ?
N21 Ni N31 93.72(14) 6_557 . ?
N21 Ni N31 90.08(14) . . ?
N24 Ni N31 168.59(14) . . ?
N24 Ni N31 95.07(14) 6_557 . ?
N31 Ni N31 89.1(2) 6_557 . ?
O13 Cl1 O14 108.7(6) . . ?
O13 Cl1 O11 110.4(7) . . ?
O14 Cl1 O11 107.8(6) . . ?
O13 Cl1 O12 114.9(6) . . ?
O14 Cl1 O12 103.7(4) . . ?
O11 Cl1 O12 110.9(6) . . ?
O13 O13 Cl1 144.1(5) 6_557 . ?
O21 Cl2 O21 118.6(10) 5_556 . ?
O21 Cl2 O22 105.5(4) 5_556 5_556 ?
O21 Cl2 O22 108.1(4) . 5_556 ?
O21 Cl2 O22 108.1(4) 5_556 . ?
O21 Cl2 O22 105.5(4) . . ?
O22 Cl2 O22 111.0(4) 5_556 . ?
O52 N51 O53 119.1(15) . . ?
O52 N51 C54 124.3(13) . . ?
O53 N51 C54 113.5(16) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.407(6) . ?
C1 C9 1.425(6) . ?
C1 C11 1.495(6) . ?
C2 C3 1.408(6) . ?
C2 N21 1.424(5) . ?
C3 C4 1.352(7) . ?
C4 C10 1.399(7) . ?
C5 C6 1.344(9) . ?
C5 C10 1.427(7) . ?
C6 C7 1.416(7) . ?
C7 C8 1.372(7) . ?
C8 C9 1.416(7) . ?
C9 C10 1.445(7) . ?
C11 C12 1.390(6) . ?
C11 C19 1.408(7) . ?
C12 C13 1.408(7) . ?
C12 N31 1.415(6) . ?
C13 C14 1.393(8) . ?
C14 C20 1.405(7) . ?
C15 C16 1.373(8) . ?
C15 C20 1.416(7) . ?
C16 C17 1.388(8) . ?
C17 C18 1.373(8) . ?
C18 C19 1.429(6) . ?
C19 C20 1.445(6) . ?
N21 C22 1.277(6) . ?
N21 Ni 2.079(4) . ?
C22 C23 1.446(6) . ?
C23 N24 1.358(6) . ?
C23 C28 1.383(7) . ?
N24 C25 1.350(6) . ?
N24 Ni 2.106(4) . ?
C25 C26 1.387(7) . ?
C26 C27 1.348(8) . ?
C27 C28 1.404(7) . ?
N31 Ni 2.162(4) . ?
Ni N21 2.079(4) 6_557 ?
Ni N24 2.106(4) 6_557 ?
Ni N31 2.162(4) 6_557 ?
Cl1 O13 1.391(11) . ?
Cl1 O14 1.439(7) . ?
Cl1 O11 1.439(13) . ?
Cl1 O12 1.486(7) . ?
O13 O13 1.002(18) 6_557 ?
C91 O92 1.272(16) . ?
Cl2 O21 1.414(7) 5_556 ?
Cl2 O21 1.414(7) . ?
Cl2 O22 1.426(4) 5_556 ?
Cl2 O22 1.426(4) . ?
N51 O52 1.254(8) . ?
N51 O53 1.335(10) . ?
N51 C54 1.395(9) . ?
