#------------------------------------------------------------------------------
#$Date: 2023-12-06 19:45:49 +0100 (Wed 06 de Dec de 2023) $
#$Revision: 288092 $
#$URL: svn://www.crystallography.net/cod/cif/1/57/05/1570517.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_1570517
loop_
_publ_author_name
'Kosuge, Ryota'
'Kawasaki, Takeshi'
'Kitase, Kosuke'
'Kosone, Takashi'
_publ_section_title
;
 The Synthesis and Crystal Structures of New One- and Two-Dimensional
 Fe(II) Coordination Polymers Using Imidazole Derivatives
;
_journal_issue                   12
_journal_name_full               Crystals
_journal_page_first              1658
_journal_paper_doi               10.3390/cryst13121658
_journal_volume                  13
_journal_year                    2023
_chemical_formula_sum            'C28 H32 Fe N12 Ni'
_chemical_formula_weight         651.18
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                106.7710(10)
_cell_angle_beta                 105.1180(10)
_cell_angle_gamma                103.2060(10)
_cell_formula_units_Z            1
_cell_length_a                   8.8641(7)
_cell_length_b                   10.0807(10)
_cell_length_c                   10.2350(10)
_cell_measurement_reflns_used    1402
_cell_measurement_temperature    275(2)
_cell_measurement_theta_max      24.9692
_cell_measurement_theta_min      2.2341
_cell_volume                     798.42(13)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      275(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5661
_diffrn_reflns_theta_full        28.67
_diffrn_reflns_theta_max         28.67
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    1.082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pillar
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.330
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.747
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         4042
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.747
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1000P)²+0.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1299
_reflns_number_gt                2925
_reflns_number_total             4042
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Compound3.cif
_cod_data_source_block           201115Ni_Allyl
_cod_database_code               1570517
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni1 0.5 0.5 1.0 0.02938(14) Uani d . P S 1 . .
Fe Fe1 0.5 0.5 0.5 0.02707(14) Uani d . P S 1 . .
N N5 0.6288(3) 0.7337(2) 0.6255(2) 0.0342(5) Uani d . . . 1 . .
N N1 0.4559(3) 0.4726(2) 0.6908(2) 0.0369(5) Uani d . . . 1 . .
N N3 0.7246(3) 0.4407(2) 0.5568(2) 0.0377(5) Uani d . . . 1 . .
N N6 0.7435(3) 0.9483(2) 0.8071(3) 0.0402(5) Uani d . . . 1 . .
N N4 0.9032(3) 0.3272(3) 0.5187(3) 0.0470(6) Uani d . . . 1 . .
C C1 0.4691(3) 0.4800(3) 0.8075(3) 0.0331(5) Uani d . . . 1 . .
C C2 0.7014(4) 0.6490(3) 1.0573(3) 0.0387(6) Uani d . . . 1 . .
C C14 0.6933(3) 0.8014(3) 0.7679(3) 0.0387(6) Uani d . . . 1 . .
H H14 0.70315 0.753723 0.833475 0.046 Uiso calc U . R 1 . .
N N2 0.8238(3) 0.7393(3) 1.0898(3) 0.0560(7) Uani d . . . 1 . .
C C8 0.7872(4) 0.3788(3) 0.4609(3) 0.0428(6) Uani d . . . 1 . .
H H8 0.754242 0.372054 0.364542 0.051 Uiso calc U . R 1 . .
C C9 0.6382(4) 0.8435(3) 0.5709(3) 0.0448(7) Uani d . . . 1 . .
H H9 0.602098 0.829115 0.472482 0.054 Uiso calc U . R 1 . .
C C11 0.8202(4) 1.0575(3) 0.9567(4) 0.0521(8) Uani d . . . 1 . .
H H11A 0.931519 1.114153 0.970944 0.063 Uiso calc U . R 1 . .
H H11B 0.828109 1.007168 1.024678 0.063 Uiso calc U . R 1 . .
C C10 0.7078(4) 0.9755(3) 0.6813(4) 0.0506(7) Uani d . . . 1 . .
H H10 0.727459 1.066934 0.673217 0.061 Uiso calc U . R 1 . .
C C3 0.8067(4) 0.4253(4) 0.6829(3) 0.0496(7) Uani d . . . 1 . .
H H3 0.789196 0.457866 0.77068 0.06 Uiso calc U . R 1 . .
C C4 0.9161(4) 0.3559(4) 0.6602(4) 0.0555(8) Uani d . . . 1 . .
H H4 0.986631 0.332318 0.728016 0.067 Uiso calc U . R 1 . .
C C6 0.8913(5) 0.0878(4) 0.3551(4) 0.0624(9) Uani d . . . 1 . .
H H6 0.945316 0.029197 0.311598 0.075 Uiso calc U . R 1 . .
C C5 0.9908(4) 0.2460(4) 0.4420(5) 0.0699(11) Uani d . . . 1 . .
H H5A 1.09209 0.252202 0.512423 0.084 Uiso calc U . R 1 . .
H H5B 1.021136 0.291872 0.37706 0.084 Uiso calc U . R 1 . .
C C7 0.7388(6) 0.0242(4) 0.3343(5) 0.0721(11) Uani d . . . 1 . .
H H7A 0.679123 0.077872 0.37546 0.086 Uiso calc U . R 1 . .
H H7B 0.688352 -0.075288 0.278195 0.086 Uiso calc U . R 1 . .
C C12 0.7252(5) 1.1581(5) 0.9884(4) 0.0766(12) Uani d . . . 1 . .
H H12 0.615987 1.119169 0.980536 0.092 Uiso calc U . R 1 . .
C C13 0.7887(9) 1.2981(6) 1.0266(6) 0.122(2) Uani d . . . 1 . .
H H13A 0.89776 1.338756 1.034988 0.147 Uiso calc U . R 1 . .
H H13B 0.725516 1.358271 1.045787 0.147 Uiso calc U . R 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'
Fe Fe 0.3463 0.8444 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 Ni1 C1 2_667 . 180.0 ?
C1 Ni1 C2 2_667 2_667 88.75(11) ?
C1 Ni1 C2 . 2_667 91.25(11) ?
C1 Ni1 C2 2_667 . 91.25(11) ?
C1 Ni1 C2 . . 88.75(11) ?
C2 Ni1 C2 2_667 . 180.0 ?
N1 Fe1 N1 . 2_666 180.0 ?
N1 Fe1 N5 . . 89.77(8) ?
N1 Fe1 N5 2_666 . 90.23(8) ?
N1 Fe1 N5 . 2_666 90.23(8) ?
N1 Fe1 N5 2_666 2_666 89.77(8) ?
N5 Fe1 N5 . 2_666 180.0 ?
N1 Fe1 N3 . 2_666 90.28(9) ?
N1 Fe1 N3 2_666 2_666 89.72(9) ?
N5 Fe1 N3 . 2_666 86.19(8) ?
N5 Fe1 N3 2_666 2_666 93.81(8) ?
N1 Fe1 N3 . . 89.72(9) ?
N1 Fe1 N3 2_666 . 90.28(9) ?
N5 Fe1 N3 . . 93.80(8) ?
N5 Fe1 N3 2_666 . 86.19(8) ?
N3 Fe1 N3 2_666 . 180.0 ?
C14 N5 C9 . . 105.2(2) ?
C14 N5 Fe1 . . 128.29(17) ?
C9 N5 Fe1 . . 125.97(18) ?
C1 N1 Fe1 . . 164.3(2) ?
C8 N3 C3 . . 104.5(2) ?
C8 N3 Fe1 . . 124.16(19) ?
C3 N3 Fe1 . . 129.8(2) ?
C14 N6 C10 . . 106.7(2) ?
C14 N6 C11 . . 126.4(2) ?
C10 N6 C11 . . 126.9(2) ?
C8 N4 C4 . . 107.0(2) ?
C8 N4 C5 . . 126.4(3) ?
C4 N4 C5 . . 126.4(3) ?
N1 C1 Ni1 . . 177.1(2) ?
N2 C2 Ni1 . . 178.8(2) ?
N5 C14 N6 . . 111.8(2) ?
N5 C14 H14 . . 124.1 ?
N6 C14 H14 . . 124.1 ?
N3 C8 N4 . . 112.1(3) ?
N3 C8 H8 . . 124.0 ?
N4 C8 H8 . . 124.0 ?
C10 C9 N5 . . 109.9(3) ?
C10 C9 H9 . . 125.0 ?
N5 C9 H9 . . 125.0 ?
N6 C11 C12 . . 112.2(3) ?
N6 C11 H11A . . 109.2 ?
C12 C11 H11A . . 109.2 ?
N6 C11 H11B . . 109.2 ?
C12 C11 H11B . . 109.2 ?
H11A C11 H11B . . 107.9 ?
C9 C10 N6 . . 106.5(2) ?
C9 C10 H10 . . 126.8 ?
N6 C10 H10 . . 126.8 ?
C4 C3 N3 . . 110.0(3) ?
C4 C3 H3 . . 125.0 ?
N3 C3 H3 . . 125.0 ?
C3 C4 N4 . . 106.5(3) ?
C3 C4 H4 . . 126.8 ?
N4 C4 H4 . . 126.8 ?
C7 C6 C5 . . 126.9(3) ?
C7 C6 H6 . . 116.6 ?
C5 C6 H6 . . 116.6 ?
N4 C5 C6 . . 113.3(3) ?
N4 C5 H5A . . 108.9 ?
C6 C5 H5A . . 108.9 ?
N4 C5 H5B . . 108.9 ?
C6 C5 H5B . . 108.9 ?
H5A C5 H5B . . 107.7 ?
C6 C7 H7A . . 120.0 ?
C6 C7 H7B . . 120.0 ?
H7A C7 H7B . . 120.0 ?
C13 C12 C11 . . 122.2(5) ?
C13 C12 H12 . . 118.9 ?
C11 C12 H12 . . 118.9 ?
C12 C13 H13A . . 120.0 ?
C12 C13 H13B . . 120.0 ?
H13A C13 H13B . . 120.0 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 C1 2_667 1.860(2) ?
Ni1 C1 . 1.860(2) ?
Ni1 C2 2_667 1.873(3) ?
Ni1 C2 . 1.873(3) ?
Fe1 N1 . 2.169(2) ?
Fe1 N1 2_666 2.169(2) ?
Fe1 N5 . 2.183(2) ?
Fe1 N5 2_666 2.183(2) ?
Fe1 N3 2_666 2.191(2) ?
Fe1 N3 . 2.191(2) ?
N5 C14 . 1.315(3) ?
N5 C9 . 1.373(3) ?
N1 C1 . 1.148(3) ?
N3 C8 . 1.322(3) ?
N3 C3 . 1.377(4) ?
N6 C14 . 1.347(3) ?
N6 C10 . 1.366(4) ?
N6 C11 . 1.470(4) ?
N4 C8 . 1.336(4) ?
N4 C4 . 1.360(4) ?
N4 C5 . 1.459(4) ?
C2 N2 . 1.141(4) ?
C14 H14 . 0.93 ?
C8 H8 . 0.93 ?
C9 C10 . 1.349(4) ?
C9 H9 . 0.93 ?
C11 C12 . 1.478(5) ?
C11 H11A . 0.97 ?
C11 H11B . 0.97 ?
C10 H10 . 0.93 ?
C3 C4 . 1.348(4) ?
C3 H3 . 0.93 ?
C4 H4 . 0.93 ?
C6 C7 . 1.288(5) ?
C6 C5 . 1.498(5) ?
C6 H6 . 0.93 ?
C5 H5A . 0.97 ?
C5 H5B . 0.97 ?
C7 H7A . 0.93 ?
C7 H7B . 0.93 ?
C12 C13 . 1.290(6) ?
C12 H12 . 0.93 ?
C13 H13A . 0.93 ?
C13 H13B . 0.93 ?
