#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:59:37 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179165 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/26/4312675.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_4312675
loop_
_publ_author_name
'Suman Mukhopadhyay'
'Debdas Mandal'
'Dipesh Ghosh'
'Israel Goldberg'
'Muktimoy Chaudhury'
_publ_section_title
;
 Equilibrium Studies in Solution Involving Nickel(II) Complexes of
 Flexidentate Schiff Base Ligands: Isolation and Structural
 Characterization of the Planar Red and Octahedral Green Species Involved
 in the Equilibrium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8439
_journal_page_last               8445
_journal_paper_doi               10.1021/ic0346174
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C37 H38 B N3 Ni O'
_chemical_formula_weight         610.22
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.6550(10)
_cell_angle_beta                 99.3440(10)
_cell_angle_gamma                110.5200(10)
_cell_formula_units_Z            2
_cell_length_a                   9.6549(5)
_cell_length_b                   9.7345(5)
_cell_length_c                   18.0363(9)
_cell_measurement_temperature    566(2)
_cell_volume                     1526.57(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      566(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11728
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.6953
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            0.35
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         7308
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0505P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1018
_reflns_number_gt                5559
_reflns_number_total             7308
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0346174si20030604_081154_1.cif
_cod_data_source_block           Compound-1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1526.57(13)
_cod_database_code               4312675
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Ni Ni 0.90566(3) 0.40545(3) 0.319693(15) 0.03954(9) Uani 1 1 d . . .
O1 O 0.94242(16) 0.59328(15) 0.37277(8) 0.0507(4) Uani 1 1 d . . .
N1 N 0.81024(18) 0.30253(18) 0.38544(10) 0.0435(4) Uani 1 1 d . . .
N2 N 0.86412(18) 0.22048(18) 0.25377(10) 0.0479(4) Uani 1 1 d . . .
N3 N 1.01447(19) 0.4622(2) 0.24111(10) 0.0531(5) Uani 1 1 d . . .
H3B H 1.0650 0.5633 0.2482 0.075(8) Uiso 1 1 calc R . .
C1 C 0.7966(2) 0.5140(2) 0.46594(12) 0.0465(5) Uani 1 1 d . . .
C2 C 0.8773(2) 0.6225(2) 0.42834(12) 0.0435(5) Uani 1 1 d . . .
C3 C 0.8878(3) 0.7708(3) 0.45214(14) 0.0573(6) Uani 1 1 d . . .
H3A H 0.9405 0.8444 0.4283 0.056(6) Uiso 1 1 calc R . .
C4 C 0.8224(3) 0.8096(3) 0.50942(15) 0.0666(7) Uani 1 1 d . . .
H4A H 0.8308 0.9086 0.5236 0.065(7) Uiso 1 1 calc R . .
C5 C 0.7440(3) 0.7039(3) 0.54651(15) 0.0709(7) Uani 1 1 d . . .
H5A H 0.6997 0.7312 0.5853 0.087(9) Uiso 1 1 calc R . .
C6 C 0.7323(3) 0.5591(3) 0.52565(14) 0.0655(7) Uani 1 1 d . . .
H6A H 0.6808 0.4882 0.5512 0.076(8) Uiso 1 1 calc R . .
C7 C 0.7743(2) 0.3598(2) 0.44482(13) 0.0516(5) Uani 1 1 d . . .
H7A H 0.7312 0.2965 0.4758 0.073(7) Uiso 1 1 calc R . .
C8 C 0.7862(3) 0.1414(2) 0.36692(14) 0.0603(6) Uani 1 1 d . . .
H8A H 0.6988 0.0821 0.3843 0.072(7) Uiso 1 1 calc R . .
H8B H 0.8748 0.1266 0.3923 0.093(9) Uiso 1 1 calc R . .
C9 C 0.7596(3) 0.0938(2) 0.28015(15) 0.0631(6) Uani 1 1 d . . .
H9A H 0.7803 0.0039 0.2666 0.071(7) Uiso 1 1 calc R . .
H9B H 0.6547 0.0722 0.2558 0.088(9) Uiso 1 1 calc R . .
C10 C 0.7969(3) 0.2383(3) 0.17636(13) 0.0595(6) Uani 1 1 d . . .
H10A H 0.6935 0.2316 0.1736 0.069(7) Uiso 1 1 calc R . .
H10B H 0.7957 0.1602 0.1356 0.065(7) Uiso 1 1 calc R . .
C11 C 0.8972(3) 0.3929(3) 0.16794(14) 0.0676(7) Uani 1 1 d . . .
H11A H 0.9442 0.3834 0.1248 0.092(9) Uiso 1 1 calc R . .
H11B H 0.8378 0.4537 0.1594 0.098(10) Uiso 1 1 calc R . .
C12 C 1.0189(3) 0.2198(3) 0.25288(17) 0.0663(7) Uani 1 1 d . . .
H12A H 1.0138 0.1451 0.2092 0.063(7) Uiso 1 1 calc R . .
H12B H 1.0615 0.1975 0.2999 0.076(8) Uiso 1 1 calc R . .
C13 C 1.1155(3) 0.3779(3) 0.24644(17) 0.0736(8) Uani 1 1 d . . .
H13A H 1.1994 0.4269 0.2914 0.089(9) Uiso 1 1 calc R . .
H13B H 1.1565 0.3731 0.2009 0.083(8) Uiso 1 1 calc R . .
C1A C 0.93414(19) 0.14230(19) -0.17849(10) 0.0340(4) Uani 1 1 d . . .
C2A C 1.0221(2) 0.1383(2) -0.11008(12) 0.0497(5) Uani 1 1 d . . .
H2AA H 0.9732 0.1021 -0.0725 0.057(6) Uiso 1 1 calc R . .
C3A C 1.1795(2) 0.1858(3) -0.09537(13) 0.0549(6) Uani 1 1 d . . .
H3AA H 1.2328 0.1787 -0.0493 0.069(7) Uiso 1 1 calc R . .
C4A C 1.2568(2) 0.2432(2) -0.14852(13) 0.0497(5) Uani 1 1 d . . .
H4AA H 1.3621 0.2755 -0.1388 0.063(7) Uiso 1 1 calc R . .
C5A C 1.1760(2) 0.2518(2) -0.21557(13) 0.0499(5) Uani 1 1 d . . .
H5AA H 1.2266 0.2914 -0.2519 0.062(7) Uiso 1 1 calc R . .
C6A C 1.0176(2) 0.2018(2) -0.23047(12) 0.0397(4) Uani 1 1 d . . .
H6AA H 0.9656 0.2085 -0.2771 0.040(5) Uiso 1 1 calc R . .
C1B C 0.66944(18) -0.0949(2) -0.19614(11) 0.0345(4) Uani 1 1 d . . .
C2B C 0.5713(2) -0.2016(2) -0.26183(12) 0.0440(5) Uani 1 1 d . . .
H2BA H 0.5495 -0.1689 -0.3066 0.058(7) Uiso 1 1 calc R . .
C3B C 0.5046(2) -0.3546(2) -0.26335(15) 0.0550(6) Uani 1 1 d . . .
H3BA H 0.4404 -0.4213 -0.3086 0.058(6) Uiso 1 1 calc R . .
C4B C 0.5329(2) -0.4068(2) -0.19897(15) 0.0538(6) Uani 1 1 d . . .
H4BA H 0.4882 -0.5088 -0.1999 0.050(6) Uiso 1 1 calc R . .
C5B C 0.6281(2) -0.3072(2) -0.13255(14) 0.0509(5) Uani 1 1 d . . .
H5BA H 0.6487 -0.3415 -0.0882 0.060(7) Uiso 1 1 calc R . .
C6B C 0.6934(2) -0.1550(2) -0.13196(12) 0.0452(5) Uani 1 1 d . . .
H6BA H 0.7566 -0.0896 -0.0862 0.049(6) Uiso 1 1 calc R . .
C1C C 0.71527(19) 0.1821(2) -0.11644(10) 0.0345(4) Uani 1 1 d . . .
C2C C 0.5964(2) 0.1232(2) -0.08098(11) 0.0410(4) Uani 1 1 d . . .
H2CA H 0.5348 0.0215 -0.0976 0.041(5) Uiso 1 1 calc R . .
C3C C 0.5657(2) 0.2090(3) -0.02217(12) 0.0503(5) Uani 1 1 d . . .
H3CA H 0.4861 0.1641 0.0003 0.056(6) Uiso 1 1 calc R . .
C4C C 0.6527(3) 0.3608(3) 0.00298(12) 0.0554(6) Uani 1 1 d . . .
H4CA H 0.6310 0.4198 0.0413 0.063(7) Uiso 1 1 calc R . .
C5C C 0.7722(3) 0.4231(3) -0.02968(13) 0.0558(6) Uani 1 1 d . . .
H5CA H 0.8327 0.5252 -0.0130 0.077(8) Uiso 1 1 calc R . .
C6C C 0.8031(2) 0.3354(2) -0.08708(12) 0.0473(5) Uani 1 1 d . . .
H6CA H 0.8863 0.3804 -0.1072 0.060(6) Uiso 1 1 calc R . .
C1D C 0.67422(18) 0.12897(19) -0.26976(10) 0.0336(4) Uani 1 1 d . . .
C2D C 0.5875(2) 0.2179(2) -0.27085(12) 0.0414(4) Uani 1 1 d . . .
H2DA H 0.5718 0.2587 -0.2244 0.052(6) Uiso 1 1 calc R . .
C3D C 0.5239(2) 0.2478(2) -0.33816(13) 0.0509(5) Uani 1 1 d . . .
H3DA H 0.4667 0.3072 -0.3360 0.066(7) Uiso 1 1 calc R . .
C4D C 0.5446(2) 0.1906(2) -0.40772(13) 0.0523(5) Uani 1 1 d . . .
H4DA H 0.5016 0.2104 -0.4528 0.069(7) Uiso 1 1 calc R . .
C5D C 0.6305(2) 0.1029(2) -0.40983(12) 0.0503(5) Uani 1 1 d . . .
H5DA H 0.6466 0.0640 -0.4565 0.053(6) Uiso 1 1 calc R . .
C6D C 0.6925(2) 0.0735(2) -0.34238(11) 0.0421(4) Uani 1 1 d . . .
H6DA H 0.7492 0.0137 -0.3453 0.041(5) Uiso 1 1 calc R . .
B B 0.7473(2) 0.0887(2) -0.19111(12) 0.0322(4) Uani 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'
B B 0.0013 0.0007 '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'
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
O1 Ni N1 97.21(7) . . ?
O1 Ni N2 172.88(7) . . ?
N1 Ni N2 88.62(7) . . ?
O1 Ni N3 98.00(7) . . ?
N1 Ni N3 163.79(7) . . ?
N2 Ni N3 76.65(8) . . ?
C2 O1 Ni 124.41(13) . . ?
C7 N1 C8 121.51(18) . . ?
C7 N1 Ni 126.00(15) . . ?
C8 N1 Ni 112.35(13) . . ?
C9 N2 C12 116.14(18) . . ?
C9 N2 C10 113.46(17) . . ?
C12 N2 C10 108.23(18) . . ?
C9 N2 Ni 110.80(13) . . ?
C12 N2 Ni 103.49(13) . . ?
C10 N2 Ni 103.55(13) . . ?
C13 N3 C11 108.6(2) . . ?
C13 N3 Ni 101.58(15) . . ?
C11 N3 Ni 104.32(13) . . ?
C2 C1 C6 119.1(2) . . ?
C2 C1 C7 122.32(18) . . ?
C6 C1 C7 118.6(2) . . ?
O1 C2 C3 118.35(19) . . ?
O1 C2 C1 124.17(18) . . ?
C3 C2 C1 117.49(19) . . ?
C4 C3 C2 121.7(2) . . ?
C3 C4 C5 120.9(2) . . ?
C6 C5 C4 119.3(2) . . ?
C5 C6 C1 121.5(2) . . ?
N1 C7 C1 123.95(19) . . ?
N1 C8 C9 107.22(18) . . ?
N2 C9 C8 107.59(18) . . ?
N2 C10 C11 106.53(18) . . ?
N3 C11 C10 106.01(19) . . ?
N2 C12 C13 105.57(18) . . ?
N3 C13 C12 106.86(17) . . ?
C2A C1A C6A 114.36(16) . . ?
C2A C1A B 120.51(16) . . ?
C6A C1A B 125.03(16) . . ?
C3A C2A C1A 123.08(19) . . ?
C4A C3A C2A 120.4(2) . . ?
C5A C4A C3A 118.58(18) . . ?
C4A C5A C6A 120.69(19) . . ?
C1A C6A C5A 122.84(19) . . ?
C6B C1B C2B 114.03(17) . . ?
C6B C1B B 121.37(16) . . ?
C2B C1B B 124.56(17) . . ?
C3B C2B C1B 123.0(2) . . ?
C4B C3B C2B 120.3(2) . . ?
C3B C4B C5B 119.3(2) . . ?
C4B C5B C6B 119.6(2) . . ?
C5B C6B C1B 123.7(2) . . ?
C2C C1C C6C 114.41(17) . . ?
C2C C1C B 124.92(16) . . ?
C6C C1C B 120.50(16) . . ?
C3C C2C C1C 123.20(19) . . ?
C4C C3C C2C 120.07(19) . . ?
C5C C4C C3C 118.71(19) . . ?
C4C C5C C6C 120.4(2) . . ?
C5C C6C C1C 123.16(19) . . ?
C2D C1D C6D 114.38(17) . . ?
C2D C1D B 123.76(16) . . ?
C6D C1D B 121.85(15) . . ?
C3D C2D C1D 122.90(18) . . ?
C4D C3D C2D 120.53(19) . . ?
C3D C4D C5D 118.9(2) . . ?
C6D C5D C4D 119.8(2) . . ?
C5D C6D C1D 123.41(18) . . ?
C1C B C1D 108.82(14) . . ?
C1C B C1A 107.40(14) . . ?
C1D B C1A 110.85(14) . . ?
C1C B C1B 110.05(14) . . ?
C1D B C1B 110.17(14) . . ?
C1A B C1B 109.51(14) . . ?
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
Ni O1 1.8148(14) . ?
Ni N1 1.8232(16) . ?
Ni N2 1.8738(16) . ?
Ni N3 1.9312(17) . ?
O1 C2 1.313(2) . ?
N1 C7 1.286(3) . ?
N1 C8 1.479(3) . ?
N2 C9 1.492(3) . ?
N2 C12 1.500(2) . ?
N2 C10 1.503(3) . ?
N3 C13 1.479(3) . ?
N3 C11 1.480(3) . ?
C1 C2 1.412(3) . ?
C1 C6 1.416(3) . ?
C1 C7 1.421(3) . ?
C2 C3 1.406(3) . ?
C3 C4 1.367(3) . ?
C4 C5 1.380(4) . ?
C5 C6 1.362(3) . ?
C8 C9 1.516(3) . ?
C10 C11 1.523(3) . ?
C12 C13 1.527(3) . ?
C1A C2A 1.394(3) . ?
C1A C6A 1.395(2) . ?
C1A B 1.658(2) . ?
C2A C3A 1.390(3) . ?
C3A C4A 1.375(3) . ?
C4A C5A 1.359(3) . ?
C5A C6A 1.397(3) . ?
C1B C6B 1.396(3) . ?
C1B C2B 1.398(3) . ?
C1B B 1.660(3) . ?
C2B C3B 1.394(3) . ?
C3B C4B 1.361(3) . ?
C4B C5B 1.374(3) . ?
C5B C6B 1.389(3) . ?
C1C C2C 1.393(2) . ?
C1C C6C 1.399(3) . ?
C1C B 1.643(3) . ?
C2C C3C 1.386(3) . ?
C3C C4C 1.378(3) . ?
C4C C5C 1.372(3) . ?
C5C C6C 1.379(3) . ?
C1D C2D 1.399(2) . ?
C1D C6D 1.403(2) . ?
C1D B 1.643(3) . ?
C2D C3D 1.388(3) . ?
C3D C4D 1.369(3) . ?
C4D C5D 1.384(3) . ?
C5D C6D 1.382(3) . ?
