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#$Date: 2025-08-22 18:52:37 +0300 (Fri, 22 Aug 2025) $
#$Revision: 301865 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/63/7226312.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_7226312
loop_
_publ_author_name
'Panda, Tarun Kanti Kanti'
'Anga, Srinivas'
'Banerjee, Indrani'
'Nayek, Hari Pada'
_publ_section_title
;
 Alkali Metal Complexes Having Sterically Bulky Bis-Iminopyrrolyl Ligands
 -- Control of Dimeric to Monomeric Complex
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA13437H
_journal_year                    2016
_chemical_formula_moiety         'C32 H26 N3, 2(C4 H8 O), K '
_chemical_formula_sum            'C40 H42 K N3 O2'
_chemical_formula_weight         635.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-07-13 deposited with the CCDC.
2016-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.696(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6800(5)
_cell_length_b                   16.1870(3)
_cell_length_c                   16.4227(6)
_cell_measurement_reflns_used    4406
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      71.054
_cell_measurement_theta_min      4.371
_cell_volume                     3444.7(2)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_data_collection
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_molecular_graphics    'DIAMOND & Olex 2.1'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7159
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.054
_diffrn_reflns_theta_min         4.371
_exptl_absorpt_coefficient_mu    1.643
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68215
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.206
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       0.00162(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         3263
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0405
_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)+(0.0674P)²+1.1978P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1162
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2981
_reflns_number_total             3263
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ra13437h2.cif
_cod_data_source_block           1-K
_cod_database_code               7226312
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
K1 K 0.5000 0.18334(3) 0.7500 0.04582(18) Uani 1 2 d S T P
O1 O 0.35717(11) 0.07256(8) 0.66670(10) 0.0680(4) Uani 1 1 d . . .
N1 N 0.5000 0.34628(10) 0.7500 0.0311(3) Uani 1 2 d S T P
N2 N 0.51259(9) 0.28204(7) 0.59652(7) 0.0323(3) Uani 1 1 d . . .
C1 C 0.50954(9) 0.39650(8) 0.68707(8) 0.0296(3) Uani 1 1 d . . .
C2 C 0.50698(10) 0.48050(8) 0.70992(9) 0.0343(3) Uani 1 1 d . . .
H2 H 0.5133 0.5264 0.6779 0.041 Uiso 1 1 calc R U .
C3 C 0.52254(9) 0.35996(8) 0.61074(8) 0.0306(3) Uani 1 1 d . . .
H3 H 0.5385 0.3939 0.5710 0.037 Uiso 1 1 calc R U .
C4 C 0.53892(10) 0.24949(9) 0.52264(9) 0.0321(3) Uani 1 1 d . . .
H4 H 0.5770 0.2920 0.5028 0.039 Uiso 1 1 calc R U .
C5 C 0.61052(11) 0.17617(9) 0.55658(9) 0.0327(3) Uani 1 1 d . . .
C6 C 0.71688(12) 0.18827(9) 0.58714(11) 0.0408(4) Uani 1 1 d . . .
H6 H 0.7440 0.2401 0.5824 0.049 Uiso 1 1 calc R U .
C7 C 0.78288(12) 0.12374(11) 0.62456(11) 0.0476(4) Uani 1 1 d . . .
H7 H 0.8537 0.1328 0.6447 0.057 Uiso 1 1 calc R U .
C8 C 0.74434(12) 0.04631(10) 0.63221(10) 0.0421(4) Uani 1 1 d . . .
H8 H 0.7888 0.0032 0.6573 0.050 Uiso 1 1 calc R U .
C9 C 0.63868(12) 0.03364(10) 0.60211(11) 0.0436(4) Uani 1 1 d . . .
H9 H 0.6119 -0.0182 0.6071 0.052 Uiso 1 1 calc R U .
C10 C 0.57240(11) 0.09813(10) 0.56451(10) 0.0412(4) Uani 1 1 d . . .
H10 H 0.5016 0.0889 0.5444 0.049 Uiso 1 1 calc R U .
C11 C 0.44357(10) 0.22611(8) 0.44861(9) 0.0317(3) Uani 1 1 d . . .
C12 C 0.44846(12) 0.22656(10) 0.36527(10) 0.0402(4) Uani 1 1 d . . .
H12 H 0.5098 0.2411 0.3559 0.048 Uiso 1 1 calc R U .
C13 C 0.36302(13) 0.20559(11) 0.29602(10) 0.0444(4) Uani 1 1 d . . .
H13 H 0.3675 0.2061 0.2407 0.053 Uiso 1 1 calc R U .
C14 C 0.27101(12) 0.18388(9) 0.30865(10) 0.0406(4) Uani 1 1 d . . .
H14 H 0.2135 0.1705 0.2621 0.049 Uiso 1 1 calc R U .
C15 C 0.26571(11) 0.18234(9) 0.39133(10) 0.0386(3) Uani 1 1 d . . .
H15 H 0.2044 0.1672 0.4004 0.046 Uiso 1 1 calc R U .
C16 C 0.35112(11) 0.20321(9) 0.46095(10) 0.0351(3) Uani 1 1 d . . .
H16 H 0.3466 0.2019 0.5162 0.042 Uiso 1 1 calc R U .
C021 C 0.26911(15) -0.04814(11) 0.60389(13) 0.0551(4) Uani 1 1 d . . .
H02A H 0.2382 -0.0803 0.6391 0.066 Uiso 1 1 calc R U .
H02B H 0.2763 -0.0828 0.5580 0.066 Uiso 1 1 calc R U .
C022 C 0.37087(14) -0.01378(12) 0.65662(15) 0.0617(5) Uani 1 1 d . . .
H02C H 0.3943 -0.0406 0.7123 0.074 Uiso 1 1 calc R U .
H02D H 0.4219 -0.0228 0.6280 0.074 Uiso 1 1 calc R U .
C023 C 0.20480(15) 0.02813(12) 0.56794(13) 0.0569(5) Uani 1 1 d . . .
H02E H 0.2133 0.0455 0.5141 0.068 Uiso 1 1 calc R U .
H02F H 0.1322 0.0186 0.5593 0.068 Uiso 1 1 calc R U .
C024 C 0.24912(17) 0.08934(13) 0.63712(14) 0.0630(5) Uani 1 1 d . . .
H02G H 0.2358 0.1452 0.6150 0.076 Uiso 1 1 calc R U .
H02H H 0.2199 0.0826 0.6833 0.076 Uiso 1 1 calc R U .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 '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'
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
N1 K1 O1 131.96(3) . 2_656
N1 K1 O1 131.97(3) . .
O1 K1 O1 96.07(7) 2_656 .
N1 K1 N2 58.24(2) . .
O1 K1 N2 123.33(4) 2_656 .
O1 K1 N2 98.88(4) . .
N1 K1 N2 58.24(2) . 2_656
O1 K1 N2 98.88(4) 2_656 2_656
O1 K1 N2 123.34(4) . 2_656
N2 K1 N2 116.48(5) . 2_656
C024 O1 C022 107.90(14) . .
C024 O1 K1 123.54(12) . .
C022 O1 K1 127.79(12) . .
C1 N1 C1 106.19(16) 2_656 .
C1 N1 K1 126.91(8) 2_656 .
C1 N1 K1 126.90(8) . .
C3 N2 C4 117.60(11) . .
C3 N2 K1 113.43(8) . .
C4 N2 K1 126.23(8) . .
N1 C1 C2 110.98(12) . .
N1 C1 C3 118.98(12) . .
C2 C1 C3 130.02(12) . .
C2 C2 C1 105.91(8) 2_656 .
C2 C2 H2 127.0 2_656 .
C1 C2 H2 127.0 . .
N2 C3 C1 121.62(12) . .
N2 C3 H3 119.2 . .
C1 C3 H3 119.2 . .
N2 C4 C11 112.05(11) . .
N2 C4 C5 106.00(11) . .
C11 C4 C5 112.62(11) . .
N2 C4 H4 108.7 . .
C11 C4 H4 108.7 . .
C5 C4 H4 108.7 . .
C10 C5 C6 118.33(13) . .
C10 C5 C4 121.70(12) . .
C6 C5 C4 119.76(12) . .
C7 C6 C5 120.64(14) . .
C7 C6 H6 119.7 . .
C5 C6 H6 119.7 . .
C8 C7 C6 120.67(14) . .
C8 C7 H7 119.7 . .
C6 C7 H7 119.7 . .
C7 C8 C9 119.15(14) . .
C7 C8 H8 120.4 . .
C9 C8 H8 120.4 . .
C8 C9 C10 120.31(15) . .
C8 C9 H9 119.8 . .
C10 C9 H9 119.8 . .
C5 C10 C9 120.89(14) . .
C5 C10 H10 119.6 . .
C9 C10 H10 119.6 . .
C12 C11 C16 118.44(13) . .
C12 C11 C4 119.10(12) . .
C16 C11 C4 122.45(12) . .
C13 C12 C11 120.79(13) . .
C13 C12 H12 119.6 . .
C11 C12 H12 119.6 . .
C14 C13 C12 120.46(14) . .
C14 C13 H13 119.8 . .
C12 C13 H13 119.8 . .
C15 C14 C13 119.19(14) . .
C15 C14 H14 120.4 . .
C13 C14 H14 120.4 . .
C14 C15 C16 120.58(14) . .
C14 C15 H15 119.7 . .
C16 C15 H15 119.7 . .
C15 C16 C11 120.54(14) . .
C15 C16 H16 119.7 . .
C11 C16 H16 119.7 . .
C022 C021 C023 103.82(15) . .
C022 C021 H02A 111.0 . .
C023 C021 H02A 111.0 . .
C022 C021 H02B 111.0 . .
C023 C021 H02B 111.0 . .
H02A C021 H02B 109.0 . .
O1 C022 C021 107.44(16) . .
O1 C022 H02C 110.2 . .
C021 C022 H02C 110.2 . .
O1 C022 H02D 110.2 . .
C021 C022 H02D 110.2 . .
H02C C022 H02D 108.5 . .
C024 C023 C021 101.61(16) . .
C024 C023 H02E 111.4 . .
C021 C023 H02E 111.4 . .
C024 C023 H02F 111.4 . .
C021 C023 H02F 111.4 . .
H02E C023 H02F 109.3 . .
O1 C024 C023 104.96(15) . .
O1 C024 H02G 110.8 . .
C023 C024 H02G 110.8 . .
O1 C024 H02H 110.8 . .
C023 C024 H02H 110.8 . .
H02G C024 H02H 108.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 N1 2.6376(16) .
K1 O1 2.6816(13) 2_656
K1 O1 2.6816(13) .
K1 N2 3.0354(12) .
K1 N2 3.0355(12) 2_656
O1 C024 1.426(2) .
O1 C022 1.427(2) .
N1 C1 1.3536(16) 2_656
N1 C1 1.3536(16) .
N2 C3 1.2821(18) .
N2 C4 1.4696(17) .
C1 C2 1.4141(19) .
C1 C3 1.4476(18) .
C2 C2 1.389(3) 2_656
C2 H2 0.9300 .
C3 H3 0.9300 .
C4 C11 1.5185(19) .
C4 C5 1.5261(19) .
C4 H4 0.9800 .
C5 C10 1.389(2) .
C5 C6 1.393(2) .
C6 C7 1.389(2) .
C6 H6 0.9300 .
C7 C8 1.381(2) .
C7 H7 0.9300 .
C8 C9 1.385(2) .
C8 H8 0.9300 .
C9 C10 1.391(2) .
C9 H9 0.9300 .
C10 H10 0.9300 .
C11 C12 1.392(2) .
C11 C16 1.3936(19) .
C12 C13 1.387(2) .
C12 H12 0.9300 .
C13 C14 1.385(2) .
C13 H13 0.9300 .
C14 C15 1.383(2) .
C14 H14 0.9300 .
C15 C16 1.389(2) .
C15 H15 0.9300 .
C16 H16 0.9300 .
C021 C022 1.491(3) .
C021 C023 1.521(3) .
C021 H02A 0.9700 .
C021 H02B 0.9700 .
C022 H02C 0.9700 .
C022 H02D 0.9700 .
C023 C024 1.483(3) .
C023 H02E 0.9700 .
C023 H02F 0.9700 .
C024 H02G 0.9700 .
C024 H02H 0.9700 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C1 N1 C1 C2 0.48(7) 2_656 .
K1 N1 C1 C2 -179.52(7) . .
C1 N1 C1 C3 179.21(13) 2_656 .
K1 N1 C1 C3 -0.79(13) . .
N1 C1 C2 C2 -1.25(18) . 2_656
C3 C1 C2 C2 -179.80(13) . 2_656
C4 N2 C3 C1 -173.08(11) . .
K1 N2 C3 C1 -10.64(15) . .
N1 C1 C3 N2 8.70(17) . .
C2 C1 C3 N2 -172.85(13) . .
C3 N2 C4 C11 -106.33(14) . .
K1 N2 C4 C11 93.75(12) . .
C3 N2 C4 C5 130.45(12) . .
K1 N2 C4 C5 -29.47(13) . .
N2 C4 C5 C10 83.33(16) . .
C11 C4 C5 C10 -39.52(18) . .
N2 C4 C5 C6 -91.34(15) . .
C11 C4 C5 C6 145.81(13) . .
C10 C5 C6 C7 0.0(2) . .
C4 C5 C6 C7 174.85(14) . .
C5 C6 C7 C8 0.0(3) . .
C6 C7 C8 C9 -0.1(3) . .
C7 C8 C9 C10 0.1(2) . .
C6 C5 C10 C9 0.1(2) . .
C4 C5 C10 C9 -174.66(14) . .
C8 C9 C10 C5 -0.2(2) . .
N2 C4 C11 C12 154.24(13) . .
C5 C4 C11 C12 -86.36(16) . .
N2 C4 C11 C16 -26.47(18) . .
C5 C4 C11 C16 92.93(15) . .
C16 C11 C12 C13 0.7(2) . .
C4 C11 C12 C13 -179.99(14) . .
C11 C12 C13 C14 0.1(3) . .
C12 C13 C14 C15 -0.8(2) . .
C13 C14 C15 C16 0.7(2) . .
C14 C15 C16 C11 0.0(2) . .
C12 C11 C16 C15 -0.8(2) . .
C4 C11 C16 C15 179.95(13) . .
C024 O1 C022 C021 10.9(2) . .
K1 O1 C022 C021 -178.93(12) . .
C023 C021 C022 O1 13.0(2) . .
C022 C021 C023 C024 -30.6(2) . .
C022 O1 C024 C023 -31.2(2) . .
K1 O1 C024 C023 158.10(12) . .
C021 C023 C024 O1 37.96(19) . .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168354390
