#------------------------------------------------------------------------------
#$Date: 2019-11-07 23:00:35 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223913 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/05/7700516.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_7700516
loop_
_publ_author_name
'Uchida, Kaiji'
'Cosquer, Goulven'
'Sugisaki, Kenji'
'Matsuoka, Hideto'
'Sato, Kazunobu'
'Breedlove, Brian K.'
'Yamashita, Masahiro'
_publ_section_title
;
 Isostructural M(ii) complexes (M = Mn, Fe, Co) with field-induced slow
 magnetic relaxation for Mn and Co complexes.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12023
_journal_page_last               12030
_journal_paper_doi               10.1039/c8dt02150c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C26 H24 Mn N10 O6'
_chemical_formula_weight         627.49
_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
;
2018-05-02 deposited with the CCDC.    2019-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.348(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.507(2)
_cell_length_b                   21.925(3)
_cell_length_c                   7.0181(9)
_cell_measurement_reflns_used    2086
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.4390
_cell_measurement_theta_min      3.0130
_cell_volume                     2621.1(6)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.840
_diffrn_measurement_device
;
Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0985
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.840
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5919
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.840
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.680
_diffrn_reflns_theta_min         1.514
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41p (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_description       block
_exptl_crystal_F_000             1292
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: water,MeOH'
_refine_diff_density_max         1.350
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         3414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1232
_refine_ls_R_factor_gt           0.0730
_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)+(0.1133P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1783
_refine_ls_wR_factor_ref         0.2047
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2152
_reflns_number_total             3414
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt02150c2.cif
_cod_data_source_block           Mn-1
_cod_depositor_comments
'Adding full bibliography for 7700516--7700518.cif.'
_cod_database_code               7700516
_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
Mn1 Mn 0.5000 0.22427(3) 0.7500 0.0221(2) Uani 1 2 d S T P
O3 O 0.54791(16) 0.21449(11) 0.4913(4) 0.0288(6) Uani 1 1 d . . .
H9 H 0.5329 0.1789 0.4143 0.035 Uiso 1 1 calc R U .
O1 O 0.56135(15) 0.31663(11) 0.8364(4) 0.0296(6) Uani 1 1 d . . .
O2 O 0.44076(14) -0.10247(12) 0.6458(4) 0.0281(6) Uani 1 1 d . . .
N6 N 0.5000 0.11838(19) 0.7500 0.0221(9) Uani 1 2 d S T P
N3 N 0.5000 0.54042(19) 0.7500 0.0233(9) Uani 1 2 d S T P
N4 N 0.38547(18) 0.18604(13) 0.5650(5) 0.0252(7) Uani 1 1 d . . .
N2 N 0.63430(17) 0.54532(14) 0.8254(5) 0.0254(7) Uani 1 1 d . . .
C11 C 0.4377(2) 0.08736(16) 0.6573(5) 0.0217(7) Uani 1 1 d . . .
C14 C 0.5000 -0.0774(2) 0.7500 0.0223(10) Uani 1 2 d S T P
C7 C 0.5000 0.3443(2) 0.7500 0.0216(10) Uani 1 2 d S T P
C13 C 0.5000 -0.0074(2) 0.7500 0.0229(10) Uani 1 2 d S T P
C6 C 0.5000 0.4136(2) 0.7500 0.0218(10) Uani 1 2 d S T P
C12 C 0.4339(2) 0.02399(16) 0.6542(5) 0.0221(7) Uani 1 1 d . . .
H8 H 0.3877 0.0031 0.5888 0.026 Uiso 1 1 calc R U .
C4 C 0.5665(2) 0.50832(16) 0.7902(5) 0.0227(7) Uani 1 1 d . . .
C5 C 0.5707(2) 0.44541(16) 0.7950(5) 0.0238(8) Uani 1 1 d . . .
H4 H 0.6197 0.4248 0.8276 0.029 Uiso 1 1 calc R U .
C8 C 0.3203(2) 0.20857(17) 0.4540(6) 0.0267(8) Uani 1 1 d . . .
H5 H 0.3106 0.2508 0.4298 0.032 Uiso 1 1 calc R U .
C9 C 0.2669(2) 0.16173(18) 0.3760(6) 0.0304(9) Uani 1 1 d . . .
H6 H 0.2161 0.1662 0.2927 0.036 Uiso 1 1 calc R U .
C3 C 0.6379(2) 0.60453(17) 0.7691(6) 0.0297(9) Uani 1 1 d . . .
H1 H 0.5957 0.6285 0.6971 0.036 Uiso 1 1 calc R U .
C2 C 0.7139(2) 0.62268(19) 0.8364(6) 0.0349(10) Uani 1 1 d . . .
H2 H 0.7355 0.6618 0.8233 0.042 Uiso 1 1 calc R U .
C10 C 0.3035(2) 0.10871(17) 0.4453(6) 0.0279(8) Uani 1 1 d . . .
H7 H 0.2832 0.0686 0.4193 0.034 Uiso 1 1 calc R U .
C1 C 0.7529(2) 0.57172(19) 0.9282(6) 0.0352(10) Uani 1 1 d . . .
H3 H 0.8073 0.5712 0.9887 0.042 Uiso 1 1 calc R U .
C15 C 0.5982(3) 0.2547(2) 0.4262(7) 0.0433(11) Uani 1 1 d . . .
H10 H 0.6102 0.2387 0.3060 0.065 Uiso 1 1 calc R U .
H11 H 0.5727 0.2946 0.3996 0.065 Uiso 1 1 calc R U .
H12 H 0.6469 0.2590 0.5273 0.065 Uiso 1 1 calc R U .
N5 N 0.62507(17) 0.12435(14) 0.9409(4) 0.0225(7) Uani 1 1 d . . .
N1 N 0.29383(18) 0.52391(16) 0.5773(5) 0.0344(8) 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 0.0033 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'
N N 0.0061 0.0033 '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'
Mn Mn 0.3368 0.7283 '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
O3 Mn1 O3 168.71(14) . 2_656
O3 Mn1 N4 88.93(11) . 2_656
O3 Mn1 N4 86.93(11) 2_656 2_656
O3 Mn1 N4 86.93(11) . .
O3 Mn1 N4 88.93(11) 2_656 .
N4 Mn1 N4 136.90(15) 2_656 .
O3 Mn1 O1 93.44(9) . .
O3 Mn1 O1 96.47(10) 2_656 .
N4 Mn1 O1 83.00(10) 2_656 .
N4 Mn1 O1 140.06(10) . .
O3 Mn1 O1 96.47(10) . 2_656
O3 Mn1 O1 93.44(9) 2_656 2_656
N4 Mn1 O1 140.06(10) 2_656 2_656
N4 Mn1 O1 83.00(10) . 2_656
O1 Mn1 O1 57.24(13) . 2_656
O3 Mn1 N6 84.36(7) . .
O3 Mn1 N6 84.36(7) 2_656 .
N4 Mn1 N6 68.45(8) 2_656 .
N4 Mn1 N6 68.45(8) . .
O1 Mn1 N6 151.38(7) . .
O1 Mn1 N6 151.38(7) 2_656 .
O3 Mn1 C7 95.64(7) . .
O3 Mn1 C7 95.64(7) 2_656 .
N4 Mn1 C7 111.55(8) 2_656 .
N4 Mn1 C7 111.55(8) . .
O1 Mn1 C7 28.62(7) . .
O1 Mn1 C7 28.62(7) 2_656 .
N6 Mn1 C7 180.0 . .
C15 O3 Mn1 127.1(2) . .
C15 O3 H9 116.4 . .
Mn1 O3 H9 116.4 . .
C7 O1 Mn1 90.1(2) . .
C11 N6 C11 118.1(4) . 2_656
C11 N6 Mn1 121.0(2) . .
C11 N6 Mn1 121.0(2) 2_656 .
C4 N3 C4 116.3(4) . 2_656
C8 N4 N5 105.1(3) . 2_656
C8 N4 Mn1 136.4(3) . .
N5 N4 Mn1 118.4(2) 2_656 .
C3 N2 N1 111.9(3) . 2_656
C3 N2 C4 126.1(3) . .
N1 N2 C4 122.0(3) 2_656 .
N6 C11 C12 123.5(3) . .
N6 C11 N5 113.9(3) . 2_656
C12 C11 N5 122.5(3) . 2_656
O2 C14 O2 127.8(5) . 2_656
O2 C14 C13 116.1(2) . .
O2 C14 C13 116.1(2) 2_656 .
O1 C7 O1 122.5(5) 2_656 .
O1 C7 C6 118.8(2) 2_656 .
O1 C7 C6 118.8(2) . .
O1 C7 Mn1 61.2(2) 2_656 .
O1 C7 Mn1 61.2(2) . .
C6 C7 Mn1 180.0 . .
C12 C13 C12 120.3(5) 2_656 .
C12 C13 C14 119.9(2) 2_656 .
C12 C13 C14 119.9(2) . .
C5 C6 C5 119.9(5) 2_656 .
C5 C6 C7 120.1(2) 2_656 .
C5 C6 C7 120.1(2) . .
C13 C12 C11 117.3(3) . .
C13 C12 H8 121.4 . .
C11 C12 H8 121.4 . .
N3 C4 C5 124.9(3) . .
N3 C4 N2 113.0(3) . .
C5 C4 N2 122.1(3) . .
C4 C5 C6 117.1(3) . .
C4 C5 H4 121.5 . .
C6 C5 H4 121.5 . .
N4 C8 C9 111.2(3) . .
N4 C8 H5 124.4 . .
C9 C8 H5 124.4 . .
C10 C9 C8 105.5(3) . .
C10 C9 H6 127.2 . .
C8 C9 H6 127.2 . .
N2 C3 C2 106.5(3) . .
N2 C3 H1 126.8 . .
C2 C3 H1 126.8 . .
C3 C2 C1 105.2(4) . .
C3 C2 H2 127.4 . .
C1 C2 H2 127.4 . .
C9 C10 N5 106.7(3) . 2_656
C9 C10 H7 126.6 . .
N5 C10 H7 126.7 2_656 .
N1 C1 C2 112.9(4) 2_656 .
N1 C1 H3 123.6 2_656 .
C2 C1 H3 123.6 . .
O3 C15 H10 109.5 . .
O3 C15 H11 109.5 . .
H10 C15 H11 109.5 . .
O3 C15 H12 109.5 . .
H10 C15 H12 109.5 . .
H11 C15 H12 109.5 . .
C10 N5 N4 111.5(3) 2_656 2_656
C10 N5 C11 130.3(3) 2_656 2_656
N4 N5 C11 118.1(3) 2_656 2_656
C1 N1 N2 103.5(3) 2_656 2_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O3 2.179(3) .
Mn1 O3 2.179(3) 2_656
Mn1 N4 2.282(3) 2_656
Mn1 N4 2.282(3) .
Mn1 O1 2.307(3) .
Mn1 O1 2.307(3) 2_656
Mn1 N6 2.322(4) .
Mn1 C7 2.631(5) .
O3 C15 1.394(5) .
O3 H9 0.9500 .
O1 C7 1.260(3) .
O2 C14 1.250(3) .
N6 C11 1.323(4) .
N6 C11 1.323(4) 2_656
N3 C4 1.333(4) .
N3 C4 1.333(4) 2_656
N4 C8 1.320(5) .
N4 N5 1.365(4) 2_656
N2 C3 1.363(5) .
N2 N1 1.369(4) 2_656
N2 C4 1.412(4) .
C11 C12 1.391(5) .
C11 N5 1.410(4) 2_656
C14 O2 1.250(3) 2_656
C14 C13 1.535(7) .
C7 O1 1.260(3) 2_656
C7 C6 1.520(7) .
C13 C12 1.380(4) 2_656
C13 C12 1.380(4) .
C6 C5 1.392(4) 2_656
C6 C5 1.392(4) .
C12 H8 0.9500 .
C4 C5 1.381(5) .
C5 H4 0.9500 .
C8 C9 1.411(5) .
C8 H5 0.9500 .
C9 C10 1.362(5) .
C9 H6 0.9500 .
C3 C2 1.365(6) .
C3 H1 0.9500 .
C2 C1 1.388(6) .
C2 H2 0.9500 .
C10 N5 1.363(5) 2_656
C10 H7 0.9500 .
C1 N1 1.325(5) 2_656
C1 H3 0.9500 .
C15 H10 0.9800 .
C15 H11 0.9800 .
C15 H12 0.9800 .
N5 C10 1.363(5) 2_656
N5 N4 1.365(4) 2_656
N5 C11 1.410(4) 2_656
N1 C1 1.324(5) 2_656
N1 N2 1.369(4) 2_656
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
C11 N6 C11 C12 0.8(3) 2_656 .
Mn1 N6 C11 C12 -179.2(3) . .
C11 N6 C11 N5 -178.6(3) 2_656 2_656
Mn1 N6 C11 N5 1.4(3) . 2_656
Mn1 O1 C7 O1 0.002(1) . 2_656
Mn1 O1 C7 C6 180.000(0) . .
O2 C14 C13 C12 -173.8(2) . 2_656
O2 C14 C13 C12 6.2(2) 2_656 2_656
O2 C14 C13 C12 6.2(2) . .
O2 C14 C13 C12 -173.8(2) 2_656 .
O1 C7 C6 C5 17.5(2) 2_656 2_656
O1 C7 C6 C5 -162.5(2) . 2_656
O1 C7 C6 C5 -162.5(2) 2_656 .
O1 C7 C6 C5 17.5(2) . .
C12 C13 C12 C11 0.7(2) 2_656 .
C14 C13 C12 C11 -179.3(2) . .
N6 C11 C12 C13 -1.6(5) . .
N5 C11 C12 C13 177.8(3) 2_656 .
C4 N3 C4 C5 -0.8(3) 2_656 .
C4 N3 C4 N2 178.2(3) 2_656 .
C3 N2 C4 N3 -19.9(5) . .
N1 N2 C4 N3 160.6(3) 2_656 .
C3 N2 C4 C5 159.1(4) . .
N1 N2 C4 C5 -20.3(5) 2_656 .
N3 C4 C5 C6 1.5(5) . .
N2 C4 C5 C6 -177.4(3) . .
C5 C6 C5 C4 -0.7(2) 2_656 .
C7 C6 C5 C4 179.3(2) . .
N5 N4 C8 C9 0.2(4) 2_656 .
Mn1 N4 C8 C9 -178.7(3) . .
N4 C8 C9 C10 -0.3(5) . .
N1 N2 C3 C2 -1.7(5) 2_656 .
C4 N2 C3 C2 178.8(4) . .
N2 C3 C2 C1 1.2(5) . .
C8 C9 C10 N5 0.2(4) . 2_656
C3 C2 C1 N1 -0.3(5) . 2_656
