#------------------------------------------------------------------------------
#$Date: 2024-09-28 00:53:00 +0200 (Sat 28 de Sep de 2024) $
#$Revision: 294929 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/71/7717105.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_7717105
loop_
_publ_author_name
'Horniichuk, Oleksandr'
'Vendier, Laure'
'Salmon, Lionel'
'Bousseksou, Azzedine'
_publ_section_title
;
 Gradual spin crossover behavior encompassing room temperature in an
 Iron(II) complex based on heteroscorpionate ligand
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D4DT02244K
_journal_year                    2024
_chemical_formula_moiety         'C16 H36 N, C2 H3 N4, 3(C3 H4 N2)'
_chemical_formula_sum            'C27 H51 N11'
_chemical_formula_weight         529.79
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-97
_audit_update_record
;
2024-07-15 deposited with the CCDC.	2024-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.447(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.7821(4)
_cell_length_b                   8.2254(4)
_cell_length_c                   19.3571(7)
_cell_measurement_reflns_used    7892
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.7800
_cell_measurement_theta_min      4.5440
_cell_volume                     1557.01(11)
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12397
_diffrn_reflns_point_group_measured_fraction_full 0.668
_diffrn_reflns_point_group_measured_fraction_max 0.668
_diffrn_reflns_theta_full        66.570
_diffrn_reflns_theta_max         66.570
_diffrn_reflns_theta_min         4.522
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.561
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.183
_refine_diff_density_min         -0.151
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.1(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         3685
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0617P)²+0.1914P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.0998
_reflns_Friedel_coverage         0.336
_reflns_Friedel_fraction_full    0.337
_reflns_Friedel_fraction_max     0.337
_reflns_number_gt                3390
_reflns_number_total             3685
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt02244k2.cif
_cod_data_source_block           OH153
_cod_original_sg_symbol_Hall     ' 	P -2yc '
_cod_original_sg_symbol_H-M      'P 1 c 1 '
_cod_database_code               7717105
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7663(3) 0.8742(4) 0.29917(17) 0.0405(7) Uani 1 1 d . . . . .
H1 H 0.862241 0.858433 0.296428 0.049 Uiso 1 1 calc R U . . .
C2 C 0.6751(3) 0.8576(4) 0.24335(16) 0.0401(7) Uani 1 1 d . . . . .
H2 H 0.695025 0.829559 0.197074 0.048 Uiso 1 1 calc R U . . .
C3 C 0.5500(3) 0.8908(3) 0.27018(15) 0.0355(6) Uani 1 1 d . . . . .
H3 H 0.464500 0.890612 0.245757 0.043 Uiso 1 1 calc R U . . .
C4 C 0.8888(3) 1.1725(4) 0.58818(16) 0.0387(7) Uani 1 1 d . . . . .
H4 H 0.920511 1.211379 0.631940 0.046 Uiso 1 1 calc R U . . .
C5 C 0.9700(3) 1.1582(4) 0.53128(18) 0.0397(7) Uani 1 1 d . . . . .
H5 H 1.064601 1.182631 0.528331 0.048 Uiso 1 1 calc R U . . .
C6 C 0.8833(3) 1.1004(3) 0.47963(17) 0.0372(6) Uani 1 1 d . . . . .
H6 H 0.906517 1.077777 0.433251 0.045 Uiso 1 1 calc R U . . .
C7 C 0.2089(4) 0.9010(4) 0.77853(16) 0.0431(7) Uani 1 1 d . . . . .
H7 H 0.258028 0.901387 0.821487 0.052 Uiso 1 1 calc R U . . .
C8 C 0.0691(3) 0.8798(4) 0.77170(17) 0.0424(7) Uani 1 1 d . . . . .
H8 H 0.005895 0.863058 0.807458 0.051 Uiso 1 1 calc R U . . .
C9 C 0.0416(3) 0.8882(4) 0.70162(16) 0.0401(7) Uani 1 1 d . . . . .
H9 H -0.045597 0.878457 0.679253 0.048 Uiso 1 1 calc R U . . .
C10 C 0.2664(3) 0.9844(3) 0.47230(14) 0.0318(6) Uani 1 1 d . . . . .
H10 H 0.178581 0.991073 0.450346 0.038 Uiso 1 1 calc R U . . .
C11 C 0.4221(3) 0.9522(3) 0.54659(14) 0.0290(6) Uani 1 1 d . . . . .
C12 C 0.5529(3) 0.3763(3) 0.40393(14) 0.0283(6) Uani 1 1 d . . . . .
H12A H 0.626939 0.309012 0.424825 0.034 Uiso 1 1 calc R U . . .
H12B H 0.477044 0.302093 0.390503 0.034 Uiso 1 1 calc R U . . .
C13 C 0.6060(3) 0.4543(3) 0.33883(14) 0.0321(6) Uani 1 1 d . . . . .
H13A H 0.688487 0.519564 0.350471 0.039 Uiso 1 1 calc R U . . .
H13B H 0.535639 0.528261 0.318848 0.039 Uiso 1 1 calc R U . . .
C14 C 0.6413(3) 0.3251(4) 0.28604(15) 0.0405(7) Uani 1 1 d . . . . .
H14A H 0.707441 0.247808 0.307439 0.049 Uiso 1 1 calc R U . . .
H14B H 0.557460 0.263531 0.273258 0.049 Uiso 1 1 calc R U . . .
C15 C 0.7019(4) 0.3947(4) 0.22103(17) 0.0424(7) Uani 1 1 d . . . . .
H15A H 0.639784 0.476743 0.201203 0.064 Uiso 1 1 calc R U . . .
H15B H 0.714782 0.307341 0.187401 0.064 Uiso 1 1 calc R U . . .
H15C H 0.790422 0.445103 0.232503 0.064 Uiso 1 1 calc R U . . .
C16 C 0.4563(3) 0.3882(3) 0.51895(15) 0.0295(6) Uani 1 1 d . . . . .
H16A H 0.392003 0.304765 0.500746 0.035 Uiso 1 1 calc R U . . .
H16B H 0.537285 0.330584 0.538481 0.035 Uiso 1 1 calc R U . . .
C17 C 0.3879(3) 0.4779(3) 0.57708(15) 0.0325(6) Uani 1 1 d . . . . .
H17A H 0.301728 0.527954 0.559639 0.039 Uiso 1 1 calc R U . . .
H17B H 0.448688 0.565770 0.594599 0.039 Uiso 1 1 calc R U . . .
C18 C 0.3576(3) 0.3600(4) 0.63544(16) 0.0391(7) Uani 1 1 d . . . . .
H18A H 0.299825 0.270331 0.617032 0.047 Uiso 1 1 calc R U . . .
H18B H 0.444508 0.312275 0.653159 0.047 Uiso 1 1 calc R U . . .
C19 C 0.2851(4) 0.4416(5) 0.69459(17) 0.0508(8) Uani 1 1 d . . . . .
H19A H 0.342449 0.529445 0.713482 0.076 Uiso 1 1 calc R U . . .
H19B H 0.268226 0.361498 0.730865 0.076 Uiso 1 1 calc R U . . .
H19C H 0.197755 0.486551 0.677584 0.076 Uiso 1 1 calc R U . . .
C20 C 0.6131(3) 0.6104(3) 0.48182(14) 0.0282(6) Uani 1 1 d . . . . .
H20A H 0.638539 0.676340 0.441349 0.034 Uiso 1 1 calc R U . . .
H20B H 0.574234 0.685381 0.516179 0.034 Uiso 1 1 calc R U . . .
C21 C 0.7423(3) 0.5361(3) 0.51311(15) 0.0308(6) Uani 1 1 d . . . . .
H21A H 0.778518 0.452814 0.481507 0.037 Uiso 1 1 calc R U . . .
H21B H 0.721767 0.482829 0.557515 0.037 Uiso 1 1 calc R U . . .
C22 C 0.8487(3) 0.6701(4) 0.52508(15) 0.0348(6) Uani 1 1 d . . . . .
H22A H 0.869303 0.721418 0.480281 0.042 Uiso 1 1 calc R U . . .
H22B H 0.810049 0.754669 0.555288 0.042 Uiso 1 1 calc R U . . .
C23 C 0.9807(3) 0.6058(4) 0.55822(17) 0.0405(7) Uani 1 1 d . . . . .
H23A H 0.962263 0.563534 0.604400 0.061 Uiso 1 1 calc R U . . .
H23B H 1.047811 0.694021 0.561986 0.061 Uiso 1 1 calc R U . . .
H23C H 1.017144 0.518346 0.529618 0.061 Uiso 1 1 calc R U . . .
C24 C 0.3835(3) 0.5939(3) 0.43088(14) 0.0286(5) Uani 1 1 d . . . . .
H24A H 0.352239 0.665721 0.468376 0.034 Uiso 1 1 calc R U . . .
H24B H 0.417636 0.664548 0.393667 0.034 Uiso 1 1 calc R U . . .
C25 C 0.2612(3) 0.4997(3) 0.40258(15) 0.0318(6) Uani 1 1 d . . . . .
H25A H 0.231230 0.420272 0.437503 0.038 Uiso 1 1 calc R U . . .
H25B H 0.287451 0.438836 0.360823 0.038 Uiso 1 1 calc R U . . .
C26 C 0.1438(3) 0.6155(4) 0.38432(16) 0.0343(6) Uani 1 1 d . . . . .
H26A H 0.117934 0.676064 0.426222 0.041 Uiso 1 1 calc R U . . .
H26B H 0.174574 0.695394 0.349755 0.041 Uiso 1 1 calc R U . . .
C27 C 0.0194(3) 0.5246(4) 0.35533(19) 0.0447(7) Uani 1 1 d . . . . .
H27A H 0.042832 0.471530 0.311861 0.067 Uiso 1 1 calc R U . . .
H27B H -0.055671 0.601408 0.346838 0.067 Uiso 1 1 calc R U . . .
H27C H -0.008852 0.442194 0.388648 0.067 Uiso 1 1 calc R U . . .
N1 N 0.5708(3) 0.9235(3) 0.33724(13) 0.0341(5) Uani 1 1 d . . . . .
N2 N 0.7035(3) 0.9147(3) 0.35686(14) 0.0409(6) Uani 1 1 d . . . . .
N3 N 0.7603(3) 1.0822(3) 0.50728(12) 0.0328(5) Uani 1 1 d . . . . .
N4 N 0.7602(3) 1.1254(3) 0.57449(13) 0.0367(6) Uani 1 1 d . . . . .
N5 N 0.1603(3) 0.9127(3) 0.67126(14) 0.0366(5) Uani 1 1 d . . . . .
N6 N 0.2661(3) 0.9207(3) 0.71745(13) 0.0419(6) Uani 1 1 d . . . . .
N7 N 0.4846(2) 0.9909(3) 0.48892(12) 0.0304(5) Uani 1 1 d . . . . .
N8 N 0.3801(2) 1.0124(3) 0.43933(12) 0.0311(5) Uani 1 1 d . . . . .
N9 N 0.2843(2) 0.9452(3) 0.54023(12) 0.0319(5) Uani 1 1 d . . . . .
N10 N 0.4939(3) 0.9137(3) 0.60726(12) 0.0329(5) Uani 1 1 d . . . . .
N11 N 0.5020(2) 0.4919(3) 0.45886(12) 0.0282(5) Uani 1 1 d . . . . .
H1B H 0.506(4) 0.952(4) 0.3684(18) 0.037(9) Uiso 1 1 d . . . . .
H3X H 0.682(4) 1.042(4) 0.4908(17) 0.031(8) Uiso 1 1 d . . . . .
H5X H 0.184(5) 0.925(5) 0.624(3) 0.068(13) Uiso 1 1 d . . . . .
H10A H 0.580(4) 0.968(5) 0.6109(19) 0.049(10) Uiso 1 1 d . . . . .
H10B H 0.442(3) 0.922(3) 0.6475(17) 0.028(7) 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 0.0181 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'
N N 0.0311 0.0180 '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
N2 C1 C2 112.1(3) . . ?
C3 C2 C1 104.4(3) . . ?
N1 C3 C2 107.0(3) . . ?
N4 C4 C5 112.0(3) . . ?
C6 C5 C4 104.6(3) . . ?
N3 C6 C5 106.9(3) . . ?
N6 C7 C8 111.6(3) . . ?
C9 C8 C7 104.9(3) . . ?
N5 C9 C8 106.9(3) . . ?
N8 C10 N9 114.8(3) . . ?
N7 C11 N9 114.4(2) . . ?
N7 C11 N10 122.2(3) . . ?
N9 C11 N10 123.3(3) . . ?
C13 C12 N11 116.2(2) . . ?
C12 C13 C14 110.5(2) . . ?
C15 C14 C13 113.2(3) . . ?
C17 C16 N11 116.1(2) . . ?
C16 C17 C18 109.8(2) . . ?
C19 C18 C17 112.4(3) . . ?
C21 C20 N11 116.2(2) . . ?
C20 C21 C22 109.1(2) . . ?
C23 C22 C21 112.4(2) . . ?
C25 C24 N11 115.7(2) . . ?
C24 C25 C26 110.3(2) . . ?
C27 C26 C25 111.6(2) . . ?
C3 N1 N2 112.7(3) . . ?
C1 N2 N1 103.8(2) . . ?
C6 N3 N4 112.3(3) . . ?
C4 N4 N3 104.1(2) . . ?
C9 N5 N6 112.2(3) . . ?
C7 N6 N5 104.4(3) . . ?
C11 N7 N8 105.3(2) . . ?
C10 N8 N7 104.9(2) . . ?
C11 N9 C10 100.5(2) . . ?
C20 N11 C16 111.0(2) . . ?
C20 N11 C12 111.2(2) . . ?
C16 N11 C12 107.02(19) . . ?
C20 N11 C24 106.47(18) . . ?
C16 N11 C24 110.3(2) . . ?
C12 N11 C24 110.9(2) . . ?
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 N2 1.331(4) . ?
C1 C2 1.391(4) . ?
C2 C3 1.369(4) . ?
C3 N1 1.336(4) . ?
C4 N4 1.336(4) . ?
C4 C5 1.379(5) . ?
C5 C6 1.379(4) . ?
C6 N3 1.337(4) . ?
C7 N6 1.331(4) . ?
C7 C8 1.381(5) . ?
C8 C9 1.378(4) . ?
C9 N5 1.330(4) . ?
C10 N8 1.317(4) . ?
C10 N9 1.361(4) . ?
C11 N7 1.325(4) . ?
C11 N9 1.352(4) . ?
C11 N10 1.390(4) . ?
C12 C13 1.518(4) . ?
C12 N11 1.520(3) . ?
C13 C14 1.520(4) . ?
C14 C15 1.517(4) . ?
C16 C17 1.515(4) . ?
C16 N11 1.518(3) . ?
C17 C18 1.524(4) . ?
C18 C19 1.518(4) . ?
C20 C21 1.516(4) . ?
C20 N11 1.518(3) . ?
C21 C22 1.529(4) . ?
C22 C23 1.523(4) . ?
C24 C25 1.516(4) . ?
C24 N11 1.520(3) . ?
C25 C26 1.527(4) . ?
C26 C27 1.523(4) . ?
N1 N2 1.345(4) . ?
N3 N4 1.349(3) . ?
N5 N6 1.352(4) . ?
N7 N8 1.395(3) . ?
