#------------------------------------------------------------------------------
#$Date: 2015-06-07 02:44:10 +0300 (Sun, 07 Jun 2015) $
#$Revision: 138673 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/50/7035022.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_7035022
loop_
_publ_author_name
'Nemec, Ivan'
'Herchel, Radovan'
'Svoboda, Ingrid'
'Boča, Roman'
'Trávníček, Zdeněk'
_publ_section_title
;
 Large and negative magnetic anisotropy in pentacoordinate mononuclear
 Ni(ii) Schiff base complexes.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9551
_journal_page_last               9560
_journal_paper_doi               10.1039/c5dt00600g
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C21 H25 N3 Ni O2'
_chemical_formula_weight         410.15
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-04-08 deposited with the CCDC.
2015-04-09 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.008(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.9490(8)
_cell_length_b                   14.037(2)
_cell_length_c                   20.113(5)
_cell_measurement_reflns_used    8223
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.41
_cell_measurement_theta_min      2.93
_cell_volume                     1960.7(6)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  ' enCIFer (Allen et al., 2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_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  0.0581
_diffrn_reflns_av_unetI/netI     0.0783
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7791
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    1.010
_exptl_absorpt_correction_T_max  0.7652
_exptl_absorpt_correction_T_min  0.7188
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.880
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         3411
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.881
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0746P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1378
_reflns_number_gt                1865
_reflns_number_total             3411
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00600g2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7035019--7035022.cif.'
_cod_database_code               7035022
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3105(7) 0.3675(4) 0.3655(3) 0.0552(13) Uani 1 1 d . B .
C2 C 0.1416(7) 0.3109(4) 0.3646(3) 0.0652(15) Uani 1 1 d . . .
H2 H 0.0351 0.3299 0.3386 0.078 Uiso 1 1 calc R . .
C3 C 0.1316(9) 0.2291(4) 0.4010(3) 0.0782(18) Uani 1 1 d . . .
H3 H 0.0199 0.1927 0.3975 0.094 Uiso 1 1 calc R . .
C4 C 0.2796(10) 0.1985(4) 0.4424(3) 0.0796(18) Uani 1 1 d . . .
H4 H 0.2691 0.1427 0.4669 0.096 Uiso 1 1 calc R . .
C5 C 0.4442(9) 0.2528(4) 0.4467(3) 0.0749(17) Uani 1 1 d . . .
H5 H 0.5447 0.2336 0.4754 0.090 Uiso 1 1 calc R . .
C6 C 0.4653(7) 0.3363(4) 0.4092(2) 0.0539(13) Uani 1 1 d . . .
C7 C 0.6424(7) 0.3909(4) 0.4171(2) 0.0570(13) Uani 1 1 d . . .
H7 H 0.7267 0.3740 0.4520 0.068 Uiso 1 1 calc R . .
C8 C 0.8682(6) 0.5145(4) 0.3981(3) 0.0668(16) Uani 1 1 d D . .
H8A H 0.9484 0.5194 0.3597 0.080 Uiso 1 1 calc R A 1
H8B H 0.9415 0.4824 0.4334 0.080 Uiso 1 1 calc R A 1
C9A C 0.810(5) 0.6135(14) 0.4209(16) 0.072(4) Uani 0.460(8) 1 d PD B 1
H9A1 H 0.9074 0.6583 0.4070 0.086 Uiso 0.460(8) 1 calc PR B 1
H9A2 H 0.8128 0.6139 0.4692 0.086 Uiso 0.460(8) 1 calc PR B 1
C10A C 0.6137(15) 0.6500(9) 0.3959(5) 0.063(4) Uani 0.460(8) 1 d PD B 1
H10A H 0.5177 0.6173 0.4214 0.076 Uiso 0.460(8) 1 calc PR B 1
H10B H 0.6071 0.7168 0.4078 0.076 Uiso 0.460(8) 1 calc PR B 1
C9B C 0.826(4) 0.6202(11) 0.4105(14) 0.072(4) Uani 0.540(8) 1 d PD B 2
H9B1 H 0.7388 0.6249 0.4469 0.086 Uiso 0.540(8) 1 calc PR B 2
H9B2 H 0.9458 0.6511 0.4248 0.086 Uiso 0.540(8) 1 calc PR B 2
C10B C 0.7398(14) 0.6752(9) 0.3509(7) 0.101(5) Uani 0.540(8) 1 d PD B 2
H10C H 0.7279 0.7416 0.3635 0.121 Uiso 0.540(8) 1 calc PR B 2
H10D H 0.8297 0.6723 0.3151 0.121 Uiso 0.540(8) 1 calc PR B 2
C11A C 0.7014(17) 0.6949(9) 0.2817(6) 0.073(4) Uani 0.460(8) 1 d P B 1
H11A H 0.6679 0.6855 0.2355 0.110 Uiso 0.460(8) 1 calc PR B 1
H11B H 0.8278 0.6697 0.2913 0.110 Uiso 0.460(8) 1 calc PR B 1
H11C H 0.7002 0.7617 0.2918 0.110 Uiso 0.460(8) 1 calc PR B 1
C11B C 0.3909(14) 0.6572(8) 0.3770(6) 0.081(4) Uani 0.540(8) 1 d P B 2
H11D H 0.3797 0.7238 0.3870 0.122 Uiso 0.540(8) 1 calc PR B 2
H11E H 0.4240 0.6228 0.4170 0.122 Uiso 0.540(8) 1 calc PR B 2
H11F H 0.2703 0.6342 0.3586 0.122 Uiso 0.540(8) 1 calc PR B 2
C12A C 0.3657(14) 0.6838(8) 0.3136(6) 0.060(4) Uani 0.460(8) 1 d PD B 1
H12A H 0.3717 0.7485 0.3306 0.072 Uiso 0.460(8) 1 calc PR B 1
H12B H 0.2768 0.6492 0.3409 0.072 Uiso 0.460(8) 1 calc PR B 1
C13A C 0.275(5) 0.6884(11) 0.2433(16) 0.072(4) Uani 0.460(8) 1 d PD B 1
H13A H 0.1547 0.7231 0.2441 0.086 Uiso 0.460(8) 1 calc PR B 1
H13B H 0.3608 0.7225 0.2145 0.086 Uiso 0.460(8) 1 calc PR B 1
C12B C 0.4985(13) 0.7074(8) 0.2683(5) 0.081(4) Uani 0.540(8) 1 d PD B 2
H12C H 0.5949 0.7011 0.2348 0.098 Uiso 0.540(8) 1 calc PR B 2
H12D H 0.5040 0.7725 0.2844 0.098 Uiso 0.540(8) 1 calc PR B 2
C13B C 0.299(4) 0.6910(9) 0.2344(14) 0.072(4) Uani 0.540(8) 1 d PD B 2
H13C H 0.2032 0.7163 0.2636 0.086 Uiso 0.540(8) 1 calc PR B 2
H13D H 0.2923 0.7290 0.1940 0.086 Uiso 0.540(8) 1 calc PR B 2
C14 C 0.2387(6) 0.5890(4) 0.2157(3) 0.0657(15) Uani 1 1 d D . .
H14A H 0.1536 0.5555 0.2449 0.079 Uiso 1 1 calc R B 1
H14B H 0.1730 0.5944 0.1725 0.079 Uiso 1 1 calc R B 1
C15 C 0.4680(6) 0.5078(3) 0.1511(2) 0.0538(12) Uani 1 1 d . . .
H15 H 0.3844 0.5229 0.1155 0.065 Uiso 1 1 calc R B .
C16 C 0.6444(6) 0.4596(4) 0.1353(2) 0.0506(12) Uani 1 1 d . B .
C17 C 0.6728(8) 0.4341(4) 0.0694(3) 0.0704(15) Uani 1 1 d . . .
H17 H 0.5732 0.4444 0.0381 0.084 Uiso 1 1 calc R B .
C18 C 0.8420(9) 0.3943(4) 0.0483(3) 0.0797(18) Uani 1 1 d . B .
H18 H 0.8569 0.3788 0.0038 0.096 Uiso 1 1 calc R . .
C19 C 0.9899(8) 0.3778(4) 0.0956(3) 0.0745(17) Uani 1 1 d . . .
H19 H 1.1049 0.3506 0.0829 0.089 Uiso 1 1 calc R B .
C20 C 0.9664(7) 0.4014(4) 0.1603(3) 0.0625(14) Uani 1 1 d . B .
H20 H 1.0675 0.3901 0.1908 0.075 Uiso 1 1 calc R . .
C21 C 0.7935(6) 0.4430(3) 0.1838(2) 0.0498(12) Uani 1 1 d . . .
N1 N 0.6922(5) 0.4596(3) 0.38053(19) 0.0534(10) Uani 1 1 d . B .
N2 N 0.5523(5) 0.6423(3) 0.3251(2) 0.0588(11) Uani 1 1 d D . .
N3 N 0.4155(5) 0.5317(3) 0.20849(19) 0.0505(10) Uani 1 1 d . B .
O1 O 0.3157(4) 0.4430(3) 0.32852(17) 0.0673(10) Uani 1 1 d . . .
O2 O 0.7846(4) 0.4641(3) 0.24652(16) 0.0672(10) Uani 1 1 d . B .
Ni1 Ni 0.55394(7) 0.49944(5) 0.29518(3) 0.0451(2) Uani 1 1 d . B .
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'
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
O1 C1 C2 119.4(5)
O1 C1 C6 124.5(4)
C2 C1 C6 116.1(5)
C3 C2 C1 121.5(5)
C2 C3 C4 122.6(6)
C3 C4 C5 118.1(6)
C4 C5 C6 122.1(6)
C5 C6 C1 119.6(5)
C5 C6 C7 119.1(5)
C1 C6 C7 121.3(5)
N1 C7 C6 125.8(5)
N1 C8 C9A 108.9(13)
N1 C8 C9B 112.6(11)
C9A C8 C9B 10(3)
C8 C9A C10A 116.7(14)
N2 C10A C9A 121.2(15)
C10B C9B C8 115.5(13)
N2 C10B C9B 116.1(15)
N2 C12A C13A 120.4(16)
C14 C13A C12A 110.9(14)
N2 C12B C13B 116.3(13)
C14 C13B C12B 118.7(11)
N3 C14 C13A 113.9(13)
N3 C14 C13B 108.1(10)
C13A C14 C13B 9(3)
N3 C15 C16 126.7(4)
C17 C16 C21 119.2(4)
C17 C16 C15 118.6(4)
C21 C16 C15 122.1(4)
C18 C17 C16 123.1(5)
C17 C18 C19 118.1(5)
C20 C19 C18 120.2(5)
C19 C20 C21 123.1(5)
O2 C21 C16 124.9(4)
O2 C21 C20 118.8(4)
C16 C21 C20 116.3(4)
C7 N1 C8 119.9(4)
C7 N1 Ni1 125.0(3)
C8 N1 Ni1 115.1(3)
C12A N2 C10B 136.1(7)
C12A N2 C10A 110.8(7)
C10B N2 C10A 53.9(7)
C12A N2 C12B 55.2(6)
C10B N2 C12B 105.8(7)
C10A N2 C12B 138.3(7)
C12A N2 C11A 109.4(8)
C10B N2 C11A 56.5(7)
C10A N2 C11A 109.2(8)
C12B N2 C11A 55.9(6)
C12A N2 C11B 52.4(6)
C10B N2 C11B 111.8(8)
C10A N2 C11B 62.6(6)
C12B N2 C11B 105.1(7)
C11A N2 C11B 144.1(7)
C12A N2 Ni1 110.9(5)
C10B N2 Ni1 113.0(5)
C10A N2 Ni1 110.1(5)
C12B N2 Ni1 111.6(5)
C11A N2 Ni1 106.3(5)
C11B N2 Ni1 109.2(5)
C15 N3 C14 119.9(4)
C15 N3 Ni1 125.8(3)
C14 N3 Ni1 114.3(3)
C1 O1 Ni1 124.3(3)
C21 O2 Ni1 127.4(3)
O2 Ni1 O1 140.73(18)
O2 Ni1 N3 89.93(14)
O1 Ni1 N3 90.20(14)
O2 Ni1 N1 88.93(14)
O1 Ni1 N1 88.84(15)
N3 Ni1 N1 176.86(17)
O2 Ni1 N2 113.39(16)
O1 Ni1 N2 105.86(16)
N3 Ni1 N2 91.52(17)
N1 Ni1 N2 91.62(18)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 O1 1.296(6)
C1 C2 1.417(6)
C1 C6 1.434(7)
C2 C3 1.364(7)
C3 C4 1.370(8)
C4 C5 1.374(8)
C5 C6 1.405(7)
C6 C7 1.454(7)
C7 N1 1.267(6)
C8 N1 1.478(6)
C8 C9A 1.522(13)
C8 C9B 1.534(11)
C9A C10A 1.527(19)
C10A N2 1.476(9)
C9B C10B 1.533(18)
C10B N2 1.460(9)
C11A N2 1.563(11)
C11B N2 1.572(9)
C12A N2 1.433(9)
C12A C13A 1.53(2)
C13A C14 1.521(13)
C12B N2 1.501(10)
C12B C13B 1.541(17)
C13B C14 1.535(12)
C14 N3 1.480(5)
C15 N3 1.267(5)
C15 C16 1.445(6)
C16 C17 1.395(6)
C16 C21 1.416(6)
C17 C18 1.382(7)
C18 C19 1.396(8)
C19 C20 1.357(7)
C20 C21 1.430(6)
C21 O2 1.300(5)
N1 Ni1 2.017(4)
N2 Ni1 2.094(4)
N3 Ni1 2.013(4)
O1 Ni1 1.974(3)
O2 Ni1 1.971(3)
