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#$Date: 2024-12-06 20:20:03 +0200 (Fri, 06 Dec 2024) $
#$Revision: 296507 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/71/7717109.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_7717109
loop_
_publ_author_name
'Horniichuk, Oleksandr Ye'
'Vendier, Laure'
'Salmon, Lionel'
'Bousseksou, Azzedine'
_publ_section_title
;
 Gradual spin crossover behavior encompasing room temperature in an
 iron(II) complex based on a heteroscorpionate ligand.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17083
_journal_page_last               17096
_journal_paper_doi               10.1039/d4dt02244k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_sum            'C16 H20 B2 Fe N16'
_chemical_formula_weight         513.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-09-10 deposited with the CCDC.	2024-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.213(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.547(3)
_cell_length_b                   16.596(4)
_cell_length_c                   12.943(4)
_cell_measurement_reflns_used    9872
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.50
_cell_measurement_theta_min      2.29
_cell_volume                     2256.1(11)
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       ω-φ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'micro-focus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0860
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            60354
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.158
_diffrn_reflns_theta_min         2.001
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_T_max  0.7431
_exptl_absorpt_correction_T_min  0.6970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         5730
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0559
_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)+(0.0364P)²+1.8114P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1150
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3909
_reflns_number_total             5730
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt02244k2.cif
_cod_data_source_block           OH184AMB
_cod_depositor_comments
'Adding full bibliography for 7717105--7717112.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7717109
_shelx_shelxl_version_number     2019/3
_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+1/2, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7782(9) 0.4885(4) 0.4356(8) 0.0400(12) Uani 0.53 1 d . . P A 1
H1 H 0.822521 0.507900 0.495888 0.048 Uiso 0.53 1 calc R U P A 1
C2 C 0.7836(8) 0.4094(4) 0.4045(6) 0.0400(12) Uani 0.53 1 d . . P A 1
H2 H 0.830386 0.367765 0.437579 0.048 Uiso 0.53 1 calc R U P A 1
C3 C 0.7059(9) 0.4051(8) 0.3153(6) 0.0400(12) Uani 0.53 1 d . . P A 1
H3 H 0.688489 0.359720 0.274381 0.048 Uiso 0.53 1 calc R U P A 1
C1B C 0.7803(10) 0.5133(4) 0.4456(9) 0.0400(12) Uani 0.47 1 d . . P A 2
H1B H 0.817612 0.544468 0.499850 0.048 Uiso 0.47 1 calc R U P A 2
C2B C 0.7978(9) 0.4309(5) 0.4289(6) 0.0400(12) Uani 0.47 1 d . . P A 2
H2B H 0.849065 0.395785 0.470198 0.048 Uiso 0.47 1 calc R U P A 2
C3B C 0.7248(10) 0.4127(9) 0.3402(7) 0.0400(12) Uani 0.47 1 d . . P A 2
H3B H 0.719246 0.361473 0.311055 0.048 Uiso 0.47 1 calc R U P A 2
C4 C 0.7522(3) 0.66576(19) 0.1104(3) 0.0485(8) Uani 1 1 d . . . . .
H4A H 0.794056 0.714929 0.119071 0.058 Uiso 1 1 calc R U . . .
C5 C 0.7547(3) 0.6173(2) 0.0238(2) 0.0517(8) Uani 1 1 d . . . . .
H5A H 0.796897 0.626843 -0.035088 0.062 Uiso 1 1 calc R U . . .
C6 C 0.6816(3) 0.55235(18) 0.0437(2) 0.0424(7) Uani 1 1 d . . . . .
H6A H 0.664839 0.508555 -0.000268 0.051 Uiso 1 1 calc R U . . .
C7 C 0.3459(2) 0.62904(16) 0.3250(2) 0.0349(6) Uani 1 1 d . . . . .
C8 C 0.3280(3) 0.52264(17) 0.2366(2) 0.0393(6) Uani 1 1 d . . . . .
H8 H 0.294378 0.477363 0.201709 0.047 Uiso 1 1 calc R U . . .
C9 C 0.5717(3) 0.63638(18) 0.5698(2) 0.0467(7) Uani 1 1 d . . . . .
H9 H 0.536471 0.585150 0.561581 0.056 Uiso 1 1 calc R U . . .
C10 C 0.5817(3) 0.6789(2) 0.6621(2) 0.0575(9) Uani 1 1 d . . . . .
H10 H 0.555292 0.662907 0.725542 0.069 Uiso 1 1 calc R U . . .
C11 C 0.6389(3) 0.74972(19) 0.6392(2) 0.0489(8) Uani 1 1 d . . . . .
H11 H 0.659424 0.791513 0.685613 0.059 Uiso 1 1 calc R U . . .
C15 C 0.9487(3) 0.67852(17) 0.3607(2) 0.0381(6) Uani 1 1 d . . . . .
C16 C 0.9669(3) 0.78284(17) 0.4524(2) 0.0410(7) Uani 1 1 d . . . . .
H16 H 1.000885 0.825643 0.492139 0.049 Uiso 1 1 calc R U . . .
N1 N 0.6595(2) 0.47897(13) 0.29816(18) 0.0374(5) Uani 1 1 d . . . . .
N2 N 0.7003(2) 0.53688(15) 0.36876(18) 0.0426(6) Uani 1 1 d . . . . .
N3 N 0.6375(2) 0.56193(13) 0.13754(17) 0.0333(5) Uani 1 1 d . . . . .
N4 N 0.6817(2) 0.63282(13) 0.18011(18) 0.0376(5) Uani 1 1 d . . . . .
N5 N 0.4500(2) 0.54272(13) 0.24242(17) 0.0338(5) Uani 1 1 d . . . . .
N6 N 0.4635(2) 0.61249(13) 0.30055(18) 0.0350(5) Uani 1 1 d . . . . .
N7 N 0.2585(2) 0.57466(15) 0.28648(19) 0.0429(6) Uani 1 1 d . . . . .
N8 N 0.3175(2) 0.69497(16) 0.3808(2) 0.0531(7) Uani 1 1 d . . . . .
H4 H 0.392488 0.735220 0.407407 0.064 Uiso 1 1 d . U . . .
H5 H 0.236539 0.712910 0.405920 0.064 Uiso 1 1 d . U . . .
N9 N 0.6608(2) 0.74895(13) 0.53844(17) 0.0356(5) Uani 1 1 d . . . . .
N10 N 0.6187(2) 0.67795(13) 0.49461(17) 0.0365(5) Uani 1 1 d . . . . .
N11 N 0.6309(2) 0.83487(13) 0.3801(2) 0.0399(5) Uani 1 1 d D . . . .
N12 N 0.5867(2) 0.77798(15) 0.30967(18) 0.0414(6) Uani 1 1 d D . . . .
N13 N 0.84342(19) 0.77039(13) 0.43189(17) 0.0345(5) Uani 1 1 d . . . . .
N14 N 0.8298(2) 0.70193(14) 0.37150(18) 0.0377(5) Uani 1 1 d . . . . .
N15 N 1.0376(2) 0.72718(15) 0.4096(2) 0.0443(6) Uani 1 1 d . . . . .
N16 N 0.9781(2) 0.61067(17) 0.3075(2) 0.0617(8) Uani 1 1 d . . . . .
H3C H 1.065042 0.594666 0.297920 0.074 Uiso 1 1 d . U . . .
H6 H 0.911600 0.575430 0.280920 0.074 Uiso 1 1 d . U . . .
Fe1 Fe 0.64634(3) 0.65724(2) 0.33685(3) 0.02820(11) Uani 1 1 d . . . . .
B1 B 0.5683(3) 0.50141(18) 0.2037(3) 0.0355(7) Uani 1 1 d . . . . .
H1C H 0.543251 0.453264 0.163009 0.043 Uiso 1 1 calc R U . . .
B2 B 0.7258(3) 0.81127(19) 0.4723(3) 0.0372(7) Uani 1 1 d . . . . .
H2C H 0.751442 0.858844 0.513983 0.045 Uiso 1 1 calc R U . . .
C12 C 0.4964(9) 0.8259(5) 0.2535(8) 0.0408(11) Uani 0.48 1 d . . P B 1
H12 H 0.445454 0.806737 0.196350 0.049 Uiso 0.48 1 calc R U P B 1
C13 C 0.4885(8) 0.9046(5) 0.2894(6) 0.0408(11) Uani 0.48 1 d . . P B 1
H13 H 0.434898 0.945424 0.262237 0.049 Uiso 0.48 1 calc R U P B 1
C14 C 0.5772(9) 0.9089(6) 0.3741(7) 0.0408(11) Uani 0.48 1 d . . P B 1
H14 H 0.596080 0.952804 0.417395 0.049 Uiso 0.48 1 calc R U P B 1
C13B C 0.4810(7) 0.8838(4) 0.2608(5) 0.0408(11) Uani 0.52 1 d D . P B 2
H13B H 0.423534 0.919121 0.225923 0.049 Uiso 0.52 1 calc R U P B 2
C14B C 0.5623(8) 0.9007(5) 0.3449(5) 0.0408(11) Uani 0.52 1 d D . P B 2
H14B H 0.570565 0.951361 0.375388 0.049 Uiso 0.52 1 calc R U P B 2
C12B C 0.5002(8) 0.8042(4) 0.2370(7) 0.0408(11) Uani 0.52 1 d D . P B 2
H12B H 0.460802 0.775091 0.181654 0.049 Uiso 0.52 1 calc R U P B 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3460 0.8440 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0010 0.0010 '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
C2 C1 N2 114.0(8) . . ?
C3 C2 C1 105.1(6) . . ?
N1 C3 C2 106.2(8) . . ?
N2 C1B C2B 105.1(8) . . ?
C3B C2B C1B 106.0(7) . . ?
C2B C3B N1 112.3(9) . . ?
N4 C4 C5 111.3(3) . . ?
C6 C5 C4 104.7(3) . . ?
N3 C6 C5 108.9(3) . . ?
N6 C7 N7 113.1(2) . . ?
N6 C7 N8 123.0(3) . . ?
N7 C7 N8 123.9(2) . . ?
N5 C8 N7 112.5(2) . . ?
N10 C9 C10 111.3(3) . . ?
C11 C10 C9 104.6(3) . . ?
N9 C11 C10 108.7(3) . . ?
N14 C15 N15 113.3(2) . . ?
N14 C15 N16 123.4(3) . . ?
N15 C15 N16 123.2(2) . . ?
N13 C16 N15 112.7(3) . . ?
C3 N1 N2 116.5(4) . . ?
N2 N1 C3B 100.4(5) . . ?
C3 N1 B1 123.5(4) . . ?
N2 N1 B1 119.9(2) . . ?
C3B N1 B1 139.6(5) . . ?
C1B N2 N1 116.1(4) . . ?
N1 N2 C1 98.1(4) . . ?
C1B N2 Fe1 125.3(4) . . ?
N1 N2 Fe1 118.17(17) . . ?
C1 N2 Fe1 143.3(4) . . ?
C6 N3 N4 109.4(2) . . ?
C6 N3 B1 129.9(2) . . ?
N4 N3 B1 119.9(2) . . ?
C4 N4 N3 105.7(2) . . ?
C4 N4 Fe1 136.0(2) . . ?
N3 N4 Fe1 117.72(16) . . ?
C8 N5 N6 107.1(2) . . ?
C8 N5 B1 132.7(2) . . ?
N6 N5 B1 120.1(2) . . ?
C7 N6 N5 104.4(2) . . ?
C7 N6 Fe1 137.29(18) . . ?
N5 N6 Fe1 118.07(15) . . ?
C8 N7 C7 103.0(2) . . ?
C11 N9 N10 109.5(2) . . ?
C11 N9 B2 131.0(2) . . ?
N10 N9 B2 119.5(2) . . ?
C9 N10 N9 105.9(2) . . ?
C9 N10 Fe1 135.83(19) . . ?
N9 N10 Fe1 118.25(16) . . ?
C14 N11 N12 118.4(4) . . ?
N12 N11 C14B 101.1(4) . . ?
C14 N11 B2 121.0(4) . . ?
N12 N11 B2 120.1(2) . . ?
C14B N11 B2 138.6(4) . . ?
C12B N12 N11 114.8(4) . . ?
N11 N12 C12 97.4(4) . . ?
C12B N12 Fe1 127.2(3) . . ?
N11 N12 Fe1 117.71(17) . . ?
C12 N12 Fe1 143.5(4) . . ?
C16 N13 N14 107.0(2) . . ?
C16 N13 B2 132.1(2) . . ?
N14 N13 B2 120.5(2) . . ?
C15 N14 N13 104.4(2) . . ?
C15 N14 Fe1 137.61(19) . . ?
N13 N14 Fe1 117.55(15) . . ?
C16 N15 C15 102.5(2) . . ?
N6 Fe1 N14 179.37(9) . . ?
N6 Fe1 N2 86.23(9) . . ?
N14 Fe1 N2 93.80(9) . . ?
N6 Fe1 N10 94.01(9) . . ?
N14 Fe1 N10 86.61(9) . . ?
N2 Fe1 N10 91.33(9) . . ?
N6 Fe1 N12 92.57(9) . . ?
N14 Fe1 N12 87.42(9) . . ?
N2 Fe1 N12 177.59(9) . . ?
N10 Fe1 N12 86.67(9) . . ?
N6 Fe1 N4 87.47(9) . . ?
N14 Fe1 N4 91.91(9) . . ?
N2 Fe1 N4 86.50(9) . . ?
N10 Fe1 N4 177.29(9) . . ?
N12 Fe1 N4 95.54(9) . . ?
N1 B1 N3 107.8(2) . . ?
N1 B1 N5 108.4(2) . . ?
N3 B1 N5 109.1(2) . . ?
N11 B2 N9 108.1(2) . . ?
N11 B2 N13 109.5(2) . . ?
N9 B2 N13 107.7(2) . . ?
C13 C12 N12 114.9(7) . . ?
C14 C13 C12 104.9(6) . . ?
N11 C14 C13 104.5(7) . . ?
C14B C13B C12B 106.5(5) . . ?
C13B C14B N11 112.4(6) . . ?
N12 C12B C13B 105.2(5) . . ?
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 C2 1.376(8) . ?
C1 N2 1.393(9) . ?
C2 C3 1.355(9) . ?
C3 N1 1.331(12) . ?
C1B N2 1.305(12) . ?
C1B C2B 1.399(9) . ?
C2B C3B 1.357(10) . ?
C3B N1 1.382(12) . ?
C4 N4 1.337(4) . ?
C4 C5 1.382(5) . ?
C5 C6 1.363(4) . ?
C6 N3 1.349(3) . ?
C7 N6 1.337(3) . ?
C7 N7 1.352(4) . ?
C7 N8 1.359(4) . ?
C8 N5 1.325(3) . ?
C8 N7 1.336(4) . ?
C9 N10 1.326(4) . ?
C9 C10 1.383(4) . ?
C10 C11 1.365(4) . ?
C11 N9 1.345(4) . ?
C15 N14 1.333(3) . ?
C15 N15 1.351(4) . ?
C15 N16 1.370(4) . ?
C16 N13 1.321(3) . ?
C16 N15 1.338(4) . ?
N1 N2 1.368(3) . ?
N1 B1 1.532(4) . ?
N2 Fe1 2.107(2) . ?
N3 N4 1.363(3) . ?
N3 B1 1.545(4) . ?
N4 Fe1 2.134(2) . ?
N5 N6 1.381(3) . ?
N5 B1 1.547(4) . ?
N6 Fe1 2.080(2) . ?
N9 N10 1.364(3) . ?
N9 B2 1.542(4) . ?
N10 Fe1 2.117(2) . ?
N11 C14 1.352(10) . ?
N11 N12 1.364(3) . ?
N11 C14B 1.365(7) . ?
N11 B2 1.538(4) . ?
N12 C12B 1.323(7) . ?
N12 C12 1.393(9) . ?
N12 Fe1 2.120(3) . ?
N13 N14 1.379(3) . ?
N13 B2 1.547(4) . ?
N14 Fe1 2.082(2) . ?
C12 C13 1.392(9) . ?
C13 C14 1.377(9) . ?
C13B C14B 1.352(7) . ?
C13B C12B 1.376(6) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C11 H11 N7 0.93 2.74 3.644(4) 165.9 4_676 yes
N16 H3C N7 0.97 2.09 3.054(3) 172.5 1_655 yes
N16 H6 N2 0.95 2.67 3.337(4) 127.5 . yes
N8 H4 N10 1.07 2.72 3.391(4) 120.8 . yes
N8 H4 N12 1.07 2.60 3.359(3) 127.3 . yes
N8 H5 N15 0.99 2.12 3.056(3) 158.5 1_455 yes
C2^a H2^a N15 0.93 2.80 3.695(9) 162.2 3_766 yes
