#------------------------------------------------------------------------------
#$Date: 2023-09-20 01:51:33 +0300 (Wed, 20 Sep 2023) $
#$Revision: 286419 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/39/7713978.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_7713978
loop_
_publ_author_name
'Jia, Shuwen'
'Zhu, Xinrui'
'Li, Dongfeng'
_publ_section_title
;
 Observation of protonation-induced intra-molecular metal-to-metal charge
 transfer in cyano-bridged [Fe−CN−Mn/Ni] dinuclear complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02200E
_journal_year                    2023
_chemical_formula_moiety         'C29 H26 N5 Ni O, 2(Cl O4)'
_chemical_formula_sum            'C29 H26 Cl2 N5 Ni O9'
_chemical_formula_weight         718.16
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-04-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-04-20 deposited with the CCDC.	2023-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 120.023(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.388(4)
_cell_length_b                   12.490(2)
_cell_length_c                   12.860(2)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      62.31
_cell_measurement_theta_min      3.71
_cell_volume                     2974.4(9)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip  (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22182
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         62.316
_diffrn_reflns_theta_min         3.714
_diffrn_source_current           3.58
_diffrn_source_power             0.250421
_diffrn_source_voltage           69.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.019
_exptl_absorpt_correction_T_max  0.7521
_exptl_absorpt_correction_T_min  0.3858
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1608 before and 0.0852 after correction.
The Ratio of minimum to maximum transmission is 0.5130.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       block
_exptl_crystal_F_000             1476
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0448
_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)+(0.0790P)²+2.1857P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1236
_refine_ls_wR_factor_ref         0.1300
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3056
_reflns_number_total             3582
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt02200e2.cif
_cod_data_source_block           230329l-1
_cod_database_code               7713978
_shelx_shelxl_version_number     2018/3
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Fixed Sof: H1(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C2(H2), C4(H4), C12(H12), C10(H10), C13(H13), C1(H1A), C3(H3),
 C14(H14), C9(H9)
3.b Tetrahedral OH refined with riding coordinates:
 O1(H1)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_olex2_submission_special_instructions 'No special instructions were received'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.500000 0.29196(3) 0.250000 0.01511(15) Uani 1 2 d S T P . .
Cl1 Cl 0.36963(3) -0.07299(4) 0.22343(5) 0.02085(16) Uani 1 1 d . . . . .
O1 O 0.500000 0.12667(18) 0.250000 0.0235(5) Uani 1 2 d S T P . .
H1 H 0.521401 0.104248 0.321124 0.035 Uiso 0.5 1 calc R U P . .
N3 N 0.500000 0.4553(2) 0.250000 0.0161(5) Uani 1 2 d S T P . .
N1 N 0.56277(11) 0.28965(15) 0.16616(18) 0.0173(4) Uani 1 1 d . . . . .
N2 N 0.60303(11) 0.30084(14) 0.40554(19) 0.0173(4) Uani 1 1 d . . . . .
O2 O 0.37884(10) 0.00282(15) 0.14593(17) 0.0283(4) Uani 1 1 d . . . . .
O4 O 0.33185(11) -0.02134(14) 0.27588(19) 0.0304(4) Uani 1 1 d . . . . .
O5 O 0.32751(12) -0.16200(16) 0.15130(19) 0.0333(5) Uani 1 1 d . . . . .
C5 C 0.65003(13) 0.37652(18) 0.4111(2) 0.0169(4) Uani 1 1 d . . . . .
C11 C 0.61423(13) 0.36546(18) 0.1947(2) 0.0178(5) Uani 1 1 d . . . . .
C15 C 0.55665(14) 0.21105(19) 0.0890(2) 0.0217(5) Uani 1 1 d . . . . .
H15 H 0.521430 0.156918 0.070731 0.026 Uiso 1 1 calc R U . . .
C8 C 0.55965(13) 0.50978(18) 0.2679(2) 0.0184(5) Uani 1 1 d . . . . .
C2 C 0.68903(14) 0.2466(2) 0.6072(2) 0.0224(5) Uani 1 1 d . . . . .
H2 H 0.701084 0.200181 0.673134 0.027 Uiso 1 1 calc R U . . .
C4 C 0.71691(13) 0.39075(19) 0.5148(2) 0.0202(5) Uani 1 1 d . . . . .
H4 H 0.748948 0.444796 0.517455 0.024 Uiso 1 1 calc R U . . .
C12 C 0.65707(13) 0.3660(2) 0.1409(2) 0.0213(5) Uani 1 1 d . . . . .
H12 H 0.691387 0.421411 0.158787 0.026 Uiso 1 1 calc R U . . .
C10 C 0.500000 0.6764(3) 0.250000 0.0253(7) Uani 1 2 d S T P . .
H10 H 0.500000 0.752450 0.249998 0.030 Uiso 1 2 calc R U P . .
C13 C 0.64927(15) 0.2849(2) 0.0611(2) 0.0248(5) Uani 1 1 d . . . . .
H13 H 0.678416 0.284329 0.024604 0.030 Uiso 1 1 calc R U . . .
C1 C 0.62342(14) 0.2372(2) 0.5016(2) 0.0213(5) Uani 1 1 d . . . . .
H1A H 0.591053 0.182766 0.496751 0.026 Uiso 1 1 calc R U . . .
C6 C 0.62763(13) 0.44415(18) 0.2969(2) 0.0181(5) Uani 1 1 d . . . . .
C3 C 0.73659(14) 0.3255(2) 0.6143(2) 0.0214(5) Uani 1 1 d . . . . .
H3 H 0.781763 0.334824 0.685728 0.026 Uiso 1 1 calc R U . . .
C14 C 0.59858(15) 0.2050(2) 0.0354(2) 0.0238(5) Uani 1 1 d . . . . .
H14 H 0.592888 0.147954 -0.017433 0.029 Uiso 1 1 calc R U . . .
C9 C 0.55972(14) 0.62115(19) 0.2642(2) 0.0233(5) Uani 1 1 d . . . . .
H9 H 0.600312 0.658691 0.271285 0.028 Uiso 1 1 calc R U . . .
C7 C 0.68971(14) 0.5213(2) 0.3197(2) 0.0220(5) Uani 1 1 d . . . . .
H7A H 0.698653 0.570401 0.385112 0.033 Uiso 1 1 calc R U . . .
H7B H 0.676282 0.562382 0.246551 0.033 Uiso 1 1 calc R U . . .
H7C H 0.733564 0.479905 0.341816 0.033 Uiso 1 1 calc R U . . .
O3 O 0.43906(11) -0.10879(18) 0.31624(19) 0.0377(5) Uani 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 0.0137 0.0067 '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'
Cl Cl 0.3281 0.5435 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -1.3357 3.2904 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0389 0.0241 '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
O1 Ni1 N1 89.21(5) . . ?
O1 Ni1 N1 89.21(5) . 2_655 ?
O1 Ni1 N2 93.01(5) . 2_655 ?
O1 Ni1 N2 93.01(5) . . ?
N3 Ni1 O1 180.0 . . ?
N3 Ni1 N1 90.79(5) . 2_655 ?
N3 Ni1 N1 90.79(5) . . ?
N3 Ni1 N2 86.99(5) . . ?
N3 Ni1 N2 86.99(5) . 2_655 ?
N1 Ni1 N1 178.43(10) 2_655 . ?
N1 Ni1 N2 98.42(8) . 2_655 ?
N1 Ni1 N2 81.66(8) . . ?
N1 Ni1 N2 98.42(8) 2_655 . ?
N1 Ni1 N2 81.66(8) 2_655 2_655 ?
N2 Ni1 N2 173.98(10) 2_655 . ?
O4 Cl1 O2 109.21(11) . . ?
O4 Cl1 O5 109.35(11) . . ?
O5 Cl1 O2 108.42(12) . . ?
O3 Cl1 O2 109.49(12) . . ?
O3 Cl1 O4 109.90(13) . . ?
O3 Cl1 O5 110.44(13) . . ?
Ni1 O1 H1 109.472(5) . 2_655 ?
Ni1 O1 H1 109.5 . . ?
H1 O1 H1 141.1 . 2_655 ?
C8 N3 Ni1 120.01(14) 2_655 . ?
C8 N3 Ni1 120.01(14) . . ?
C8 N3 C8 120.0(3) 2_655 . ?
C11 N1 Ni1 119.50(15) . . ?
C15 N1 Ni1 122.24(16) . . ?
C15 N1 C11 118.2(2) . . ?
C5 N2 Ni1 118.79(15) . . ?
C1 N2 Ni1 122.97(16) . . ?
C1 N2 C5 118.2(2) . . ?
N2 C5 C4 121.2(2) . . ?
N2 C5 C6 117.5(2) . . ?
C4 C5 C6 121.3(2) . . ?
N1 C11 C12 120.9(2) . . ?
N1 C11 C6 116.93(19) . . ?
C12 C11 C6 121.9(2) . . ?
N1 C15 H15 118.1 . . ?
N1 C15 C14 123.8(2) . . ?
C14 C15 H15 118.1 . . ?
N3 C8 C6 117.8(2) . . ?
N3 C8 C9 120.7(2) . . ?
C9 C8 C6 121.5(2) . . ?
C1 C2 H2 120.8 . . ?
C3 C2 H2 120.8 . . ?
C3 C2 C1 118.3(2) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 C5 119.8(2) . . ?
C3 C4 H4 120.1 . . ?
C11 C12 H12 120.1 . . ?
C13 C12 C11 119.7(2) . . ?
C13 C12 H12 120.1 . . ?
C9 C10 H10 120.0 . . ?
C9 C10 H10 120.0 2_655 . ?
C9 C10 C9 120.1(3) . 2_655 ?
C12 C13 H13 120.3 . . ?
C14 C13 C12 119.4(2) . . ?
C14 C13 H13 120.3 . . ?
N2 C1 C2 123.7(2) . . ?
N2 C1 H1A 118.2 . . ?
C2 C1 H1A 118.2 . . ?
C5 C6 C11 107.29(18) . . ?
C8 C6 C5 109.02(18) . . ?
C8 C6 C11 112.33(19) . . ?
C8 C6 C7 109.33(19) . . ?
C7 C6 C5 109.4(2) . . ?
C7 C6 C11 109.45(19) . . ?
C2 C3 C4 118.8(2) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C15 C14 C13 117.9(2) . . ?
C15 C14 H14 121.0 . . ?
C13 C14 H14 121.0 . . ?
C8 C9 H9 120.4 . . ?
C10 C9 C8 119.1(2) . . ?
C10 C9 H9 120.4 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
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
Ni1 O1 2.064(2) . ?
Ni1 N3 2.040(3) . ?
Ni1 N1 2.101(2) . ?
Ni1 N1 2.101(2) 2_655 ?
Ni1 N2 2.111(2) 2_655 ?
Ni1 N2 2.112(2) . ?
Cl1 O2 1.4579(18) . ?
Cl1 O4 1.4386(18) . ?
Cl1 O5 1.439(2) . ?
Cl1 O3 1.434(2) . ?
O1 H1 0.8400 . ?
O1 H1 0.8400 2_655 ?
N3 C8 1.360(3) 2_655 ?
N3 C8 1.360(3) . ?
N1 C11 1.356(3) . ?
N1 C15 1.355(3) . ?
N2 C5 1.355(3) . ?
N2 C1 1.345(3) . ?
C5 C4 1.395(3) . ?
C5 C6 1.548(3) . ?
C11 C12 1.397(3) . ?
C11 C6 1.549(3) . ?
C15 H15 0.9500 . ?
C15 C14 1.379(4) . ?
C8 C6 1.543(3) . ?
C8 C9 1.392(3) . ?
C2 H2 0.9500 . ?
C2 C1 1.386(4) . ?
C2 C3 1.385(4) . ?
C4 H4 0.9500 . ?
C4 C3 1.394(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.390(3) . ?
C10 H10 0.9500 . ?
C10 C9 1.381(3) . ?
C10 C9 1.381(3) 2_655 ?
C13 H13 0.9500 . ?
C13 C14 1.386(4) . ?
C1 H1A 0.9500 . ?
C6 C7 1.545(3) . ?
C3 H3 0.9500 . ?
C14 H14 0.9500 . ?
C9 H9 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 N3 C8 C6 -4.4(2) . . . . ?
Ni1 N3 C8 C9 177.84(16) . . . . ?
Ni1 N1 C11 C12 179.75(17) . . . . ?
Ni1 N1 C11 C6 5.1(3) . . . . ?
Ni1 N1 C15 C14 -177.8(2) . . . . ?
Ni1 N2 C5 C4 175.62(16) . . . . ?
Ni1 N2 C5 C6 -6.2(3) . . . . ?
Ni1 N2 C1 C2 -175.67(18) . . . . ?
N3 C8 C6 C5 -57.8(3) . . . . ?
N3 C8 C6 C11 61.0(2) . . . . ?
N3 C8 C6 C7 -177.33(18) . . . . ?
N3 C8 C9 C10 4.3(3) . . . . ?
N1 C11 C12 C13 -3.0(4) . . . . ?
N1 C11 C6 C5 59.3(3) . . . . ?
N1 C11 C6 C8 -60.5(3) . . . . ?
N1 C11 C6 C7 177.8(2) . . . . ?
N1 C15 C14 C13 -0.8(4) . . . . ?
N2 C5 C4 C3 0.8(3) . . . . ?
N2 C5 C6 C11 -58.6(2) . . . . ?
N2 C5 C6 C8 63.3(3) . . . . ?
N2 C5 C6 C7 -177.20(19) . . . . ?
C5 N2 C1 C2 1.9(3) . . . . ?
C5 C4 C3 C2 0.7(3) . . . . ?
C11 N1 C15 C14 -1.6(4) . . . . ?
C11 C12 C13 C14 0.5(4) . . . . ?
C15 N1 C11 C12 3.5(3) . . . . ?
C15 N1 C11 C6 -171.1(2) . . . . ?
C8 N3 C8 C6 175.6(2) 2_655 . . . ?
C8 N3 C8 C9 -2.15(16) 2_655 . . . ?
C4 C5 C6 C11 119.6(2) . . . . ?
C4 C5 C6 C8 -118.5(2) . . . . ?
C4 C5 C6 C7 1.0(3) . . . . ?
C12 C11 C6 C5 -115.3(2) . . . . ?
C12 C11 C6 C8 124.9(2) . . . . ?
C12 C11 C6 C7 3.2(3) . . . . ?
C12 C13 C14 C15 1.4(4) . . . . ?
C1 N2 C5 C4 -2.0(3) . . . . ?
C1 N2 C5 C6 176.2(2) . . . . ?
C1 C2 C3 C4 -0.8(4) . . . . ?
C6 C5 C4 C3 -177.3(2) . . . . ?
C6 C11 C12 C13 171.4(2) . . . . ?
C6 C8 C9 C10 -173.42(18) . . . . ?
C3 C2 C1 N2 -0.4(4) . . . . ?
C9 C8 C6 C5 119.9(2) . . . . ?
C9 C8 C6 C11 -121.3(2) . . . . ?
C9 C8 C6 C7 0.4(3) . . . . ?
C9 C10 C9 C8 -2.09(16) 2_655 . . . ?
