#------------------------------------------------------------------------------
#$Date: 2020-03-27 03:44:23 +0200 (Fri, 27 Mar 2020) $
#$Revision: 249764 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/76/1557665.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_1557665
loop_
_publ_author_name
'Konieczny, Piotr'
'Pel̷ka, Robert'
'Masuda, Yuka'
'Sakata, Shiomi'
'Kayahara, Saori'
'Irie, Natsumi'
'Kajiwara, Takashi'
'Baran, Stanisl̷aw'
_publ_section_title
;
 Anisotropy of Spin--Lattice Relaxations in Mononuclear Tb3+
 Single-Molecule Magnets
;
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_paper_doi               10.1021/acs.jpcc.9b11057
_journal_year                    2020
_chemical_formula_sum            'C31 H38 N4 O7 Zn'
_chemical_formula_weight         644.02
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                100.424(3)
_cell_angle_beta                 106.364(3)
_cell_angle_gamma                93.104(4)
_cell_formula_units_Z            2
_cell_length_a                   9.859(3)
_cell_length_b                   11.493(3)
_cell_length_c                   15.268(5)
_cell_measurement_reflns_used    5190
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      1.4
_cell_volume                     1622.4(8)
_computing_cell_refinement       'CrystalClear ver. 1.4'
_computing_data_collection       'CrystalClear ver. 1.4'
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics    OrtepIII
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      153(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device
;
AFC11 (Right): Eulerian 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_specimen_support Fiber
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17405
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         1.420
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.807
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.935
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.016
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         9113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0567
_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)+(0.0879P)²+1.0792P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1559
_refine_ls_wR_factor_ref         0.1709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6989
_reflns_number_total             9113
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            jp9b11057_si_003.cif
_cod_data_source_block           znhl
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               1557665
_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.
;
_shelx_estimated_absorpt_t_min   0.889
_shelx_estimated_absorpt_t_max   0.938
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Zn Zn 0.80798(3) 0.02228(3) 0.80562(2) 0.02681(11) Uani 1 1 d . . . . .
O1 O 0.6162(2) 0.1176(2) 1.04543(14) 0.0332(5) Uani 1 1 d . . . . .
O2 O 0.7298(2) 0.08946(19) 0.90813(14) 0.0302(4) Uani 1 1 d . . . . .
O3 O 0.5666(2) -0.34036(18) 0.73392(16) 0.0347(5) Uani 1 1 d . . . . .
O4 O 0.7297(2) -0.14501(17) 0.76825(13) 0.0267(4) Uani 1 1 d . . . . .
O5 O 0.7988(2) -0.4966(2) 0.21660(15) 0.0368(5) Uani 1 1 d . . . . .
O6 O 0.8026(2) -0.3573(2) 0.37396(15) 0.0353(5) Uani 1 1 d . . . . .
H1 H 0.8144 -0.3161 0.4275 0.053 Uiso 1 1 calc R U . . .
N1 N 0.7395(3) 0.1504(2) 0.73746(17) 0.0323(5) Uani 1 1 d . . . . .
N2 N 0.9986(2) -0.0113(2) 0.87629(16) 0.0286(5) Uani 1 1 d . . . . .
N3 N 0.9418(3) -0.2522(2) 0.54255(17) 0.0328(5) Uani 1 1 d . . . . .
N4 N 0.9860(3) 0.0412(2) 0.70792(17) 0.0325(5) Uani 1 1 d . . . . .
C1 C 0.5484(4) 0.1255(3) 1.1172(2) 0.0391(7) Uani 1 1 d . . . . .
H2 H 0.5614 0.2082 1.1513 0.059 Uiso 1 1 calc R U . . .
H3 H 0.5907 0.0746 1.1603 0.059 Uiso 1 1 calc R U . . .
H4 H 0.4466 0.0992 1.0893 0.059 Uiso 1 1 calc R U . . .
C2 C 0.5607(3) 0.1748(2) 0.97470(19) 0.0273(5) Uani 1 1 d . . . . .
C3 C 0.4496(3) 0.2438(3) 0.9708(2) 0.0333(6) Uani 1 1 d . . . . .
H5 H 0.4061 0.2530 1.0195 0.040 Uiso 1 1 calc R U . . .
C4 C 0.4006(3) 0.3003(3) 0.8957(2) 0.0363(7) Uani 1 1 d . . . . .
H6 H 0.3230 0.3465 0.8930 0.044 Uiso 1 1 calc R U . . .
C5 C 0.4642(3) 0.2891(3) 0.8264(2) 0.0362(7) Uani 1 1 d . . . . .
H7 H 0.4310 0.3283 0.7760 0.043 Uiso 1 1 calc R U . . .
C6 C 0.5799(3) 0.2193(2) 0.8285(2) 0.0308(6) Uani 1 1 d . . . . .
C7 C 0.6280(3) 0.1578(2) 0.90225(19) 0.0261(5) Uani 1 1 d . . . . .
C8 C 0.6451(4) 0.2172(3) 0.7552(2) 0.0339(6) Uani 1 1 d . . . . .
H8 H 0.6154 0.2711 0.7151 0.041 Uiso 1 1 calc R U . . .
C9 C 0.4743(4) -0.4486(3) 0.7105(3) 0.0505(9) Uani 1 1 d . . . . .
H9 H 0.5249 -0.5156 0.6924 0.076 Uiso 1 1 calc R U . . .
H10 H 0.3907 -0.4450 0.6583 0.076 Uiso 1 1 calc R U . . .
H11 H 0.4439 -0.4596 0.7645 0.076 Uiso 1 1 calc R U . . .
C10 C 0.6860(3) -0.3277(2) 0.8086(2) 0.0287(6) Uani 1 1 d . . . . .
C11 C 0.7212(4) -0.4100(3) 0.8644(2) 0.0364(7) Uani 1 1 d . . . . .
H12 H 0.6591 -0.4807 0.8536 0.044 Uiso 1 1 calc R U . . .
C12 C 0.8492(4) -0.3887(3) 0.9371(2) 0.0404(8) Uani 1 1 d . . . . .
H13 H 0.8724 -0.4439 0.9770 0.049 Uiso 1 1 calc R U . . .
C13 C 0.9411(4) -0.2887(3) 0.9509(2) 0.0369(7) Uani 1 1 d . . . . .
H14 H 1.0295 -0.2772 0.9985 0.044 Uiso 1 1 calc R U . . .
C14 C 0.9066(3) -0.2023(3) 0.89537(18) 0.0280(6) Uani 1 1 d . . . . .
C15 C 0.7750(3) -0.2190(2) 0.82381(18) 0.0252(5) Uani 1 1 d . . . . .
C16 C 1.0180(3) -0.1069(3) 0.90819(18) 0.0302(6) Uani 1 1 d . . . . .
H15 H 1.1120 -0.1162 0.9427 0.036 Uiso 1 1 calc R U . . .
C17 C 0.7889(4) -0.5786(3) 0.1331(2) 0.0435(8) Uani 1 1 d . . . . .
H16 H 0.8581 -0.5508 0.1041 0.065 Uiso 1 1 calc R U . . .
H17 H 0.6927 -0.5850 0.0900 0.065 Uiso 1 1 calc R U . . .
H18 H 0.8091 -0.6568 0.1473 0.065 Uiso 1 1 calc R U . . .
C18 C 0.9219(3) -0.4846(2) 0.28812(19) 0.0274(5) Uani 1 1 d . . . . .
C19 C 1.0424(3) -0.5383(3) 0.2827(2) 0.0300(6) Uani 1 1 d . . . . .
H19 H 1.0425 -0.5888 0.2261 0.036 Uiso 1 1 calc R U . . .
C20 C 1.1630(3) -0.5190(3) 0.3592(2) 0.0365(7) Uani 1 1 d . . . . .
H20 H 1.2449 -0.5567 0.3549 0.044 Uiso 1 1 calc R U . . .
C21 C 1.1643(3) -0.4451(3) 0.4415(2) 0.0349(6) Uani 1 1 d . . . . .
H21 H 1.2469 -0.4325 0.4939 0.042 Uiso 1 1 calc R U . . .
C22 C 1.0436(3) -0.3886(2) 0.44811(19) 0.0278(5) Uani 1 1 d . . . . .
C23 C 0.9214(3) -0.4090(2) 0.3716(2) 0.0267(5) Uani 1 1 d . . . . .
C24 C 1.0460(3) -0.3094(3) 0.5349(2) 0.0314(6) Uani 1 1 d . . . . .
H22 H 1.1281 -0.3003 0.5874 0.038 Uiso 1 1 calc R U . . .
C25 C 0.7969(4) 0.1676(3) 0.6610(3) 0.0477(9) Uani 1 1 d . . . . .
H23 H 0.7779 0.2465 0.6459 0.057 Uiso 1 1 calc R U . . .
H24 H 0.7494 0.1059 0.6046 0.057 Uiso 1 1 calc R U . . .
C26 C 0.9550(4) 0.1597(3) 0.6891(3) 0.0449(8) Uani 1 1 d . . . . .
H25 H 0.9936 0.1752 0.6386 0.054 Uiso 1 1 calc R U . . .
H26 H 1.0022 0.2212 0.7457 0.054 Uiso 1 1 calc R U . . .
C27 C 1.1212(3) 0.0660(3) 0.8758(2) 0.0359(7) Uani 1 1 d . . . . .
H27 H 1.2096 0.0464 0.9178 0.043 Uiso 1 1 calc R U . . .
H28 H 1.1098 0.1504 0.8975 0.043 Uiso 1 1 calc R U . . .
C28 C 1.1283(3) 0.0450(3) 0.7752(2) 0.0390(7) Uani 1 1 d . . . . .
H29 H 1.1930 0.1097 0.7688 0.047 Uiso 1 1 calc R U . . .
H30 H 1.1677 -0.0311 0.7609 0.047 Uiso 1 1 calc R U . . .
C29 C 0.9557(4) -0.1727(3) 0.6317(2) 0.0373(7) Uani 1 1 d . . . . .
H31 H 1.0400 -0.1879 0.6799 0.045 Uiso 1 1 calc R U . . .
H32 H 0.8704 -0.1876 0.6519 0.045 Uiso 1 1 calc R U . . .
C30 C 0.9717(4) -0.0442(3) 0.6206(2) 0.0353(6) Uani 1 1 d . . . . .
H33 H 1.0567 -0.0305 0.5999 0.042 Uiso 1 1 calc R U . . .
H34 H 0.8876 -0.0304 0.5716 0.042 Uiso 1 1 calc R U . . .
O7 O 0.2913(5) -0.0776(5) 0.5747(4) 0.0461(12) Uani 0.5 1 d . . P . .
H35 H 0.3478 -0.1237 0.5980 0.069 Uiso 0.5 1 calc R U P . .
C31 C 0.3514(8) 0.0337(8) 0.6058(6) 0.059(2) Uani 0.5 1 d . . P . .
H36 H 0.2774 0.0874 0.6057 0.089 Uiso 0.5 1 calc R U P . .
H37 H 0.4065 0.0537 0.5652 0.089 Uiso 0.5 1 calc R U P . .
H38 H 0.4147 0.0424 0.6694 0.089 Uiso 0.5 1 calc R U P . .
O8 O 0.5366(6) -0.1839(5) 0.5923(3) 0.0524(14) Uani 0.5 1 d . . P . .
H39 H 0.4689 -0.2019 0.6124 0.079 Uiso 0.5 1 calc R U P . .
C32 C 0.5526(7) -0.2817(8) 0.5268(4) 0.0464(18) Uani 0.5 1 d . . P . .
H40 H 0.6539 -0.2902 0.5372 0.070 Uiso 0.5 1 calc R U P . .
H41 H 0.5108 -0.2685 0.4636 0.070 Uiso 0.5 1 calc R U P . .
H42 H 0.5041 -0.3544 0.5343 0.070 Uiso 0.5 1 calc R U P . .
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'
Zn Zn 0.2839 1.4301 '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
O4 Zn N2 94.02(9) . . ?
O4 Zn O2 104.80(9) . . ?
N2 Zn O2 101.55(9) . . ?
O4 Zn N1 125.69(10) . . ?
N2 Zn N1 133.64(11) . . ?
O2 Zn N1 91.18(9) . . ?
C2 O1 C1 116.8(2) . . ?
C7 O2 Zn 126.23(18) . . ?
C10 O3 C9 117.3(3) . . ?
C15 O4 Zn 119.91(18) . . ?
C18 O5 C17 117.5(2) . . ?
C8 N1 C25 118.3(3) . . ?
C8 N1 Zn 123.64(19) . . ?
C25 N1 Zn 118.0(2) . . ?
C16 N2 C27 119.8(3) . . ?
C16 N2 Zn 122.3(2) . . ?
C27 N2 Zn 117.0(2) . . ?
C24 N3 C29 118.0(3) . . ?
C30 N4 C26 110.7(3) . . ?
C30 N4 C28 110.8(2) . . ?
C26 N4 C28 112.0(3) . . ?
O1 C2 C3 124.5(2) . . ?
O1 C2 C7 114.1(2) . . ?
C3 C2 C7 121.4(3) . . ?
C2 C3 C4 120.4(3) . . ?
C5 C4 C3 120.1(3) . . ?
C4 C5 C6 121.0(3) . . ?
C7 C6 C5 119.9(3) . . ?
C7 C6 C8 122.8(3) . . ?
C5 C6 C8 117.3(3) . . ?
O2 C7 C6 124.0(2) . . ?
O2 C7 C2 118.9(2) . . ?
C6 C7 C2 117.1(2) . . ?
N1 C8 C6 127.7(3) . . ?
O3 C10 C11 124.9(3) . . ?
O3 C10 C15 113.1(2) . . ?
C11 C10 C15 122.0(3) . . ?
C10 C11 C12 119.5(3) . . ?
C13 C12 C11 120.3(3) . . ?
C12 C13 C14 121.2(3) . . ?
C13 C14 C15 119.7(3) . . ?
C13 C14 C16 116.7(3) . . ?
C15 C14 C16 123.1(2) . . ?
O4 C15 C14 125.7(3) . . ?
O4 C15 C10 117.2(3) . . ?
C14 C15 C10 117.1(2) . . ?
N2 C16 C14 124.7(3) . . ?
O5 C18 C19 125.1(2) . . ?
O5 C18 C23 114.9(2) . . ?
C19 C18 C23 120.0(3) . . ?
C18 C19 C20 120.6(3) . . ?
C21 C20 C19 120.2(3) . . ?
C20 C21 C22 120.2(3) . . ?
C23 C22 C21 119.8(3) . . ?
C23 C22 C24 120.2(3) . . ?
C21 C22 C24 120.0(3) . . ?
O6 C23 C22 122.3(2) . . ?
O6 C23 C18 118.3(3) . . ?
C22 C23 C18 119.3(2) . . ?
N3 C24 C22 122.1(3) . . ?
N1 C25 C26 110.0(3) . . ?
N4 C26 C25 110.8(3) . . ?
N2 C27 C28 107.2(2) . . ?
N4 C28 C27 111.4(2) . . ?
N3 C29 C30 109.2(2) . . ?
N4 C30 C29 112.2(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
Zn O4 1.952(2) . ?
Zn N2 1.983(2) . ?
Zn O2 1.9864(19) . ?
Zn N1 1.994(2) . ?
O1 C2 1.364(3) . ?
O1 C1 1.428(3) . ?
O2 C7 1.301(3) . ?
O3 C10 1.369(4) . ?
O3 C9 1.427(4) . ?
O4 C15 1.315(3) . ?
O5 C18 1.365(4) . ?
O5 C17 1.418(4) . ?
O6 C23 1.349(3) . ?
N1 C8 1.293(4) . ?
N1 C25 1.472(4) . ?
N2 C16 1.283(4) . ?
N2 C27 1.463(4) . ?
N3 C24 1.270(4) . ?
N3 C29 1.462(4) . ?
N4 C30 1.472(4) . ?
N4 C26 1.472(4) . ?
N4 C28 1.480(4) . ?
C2 C3 1.382(4) . ?
C2 C7 1.432(4) . ?
C3 C4 1.401(5) . ?
C4 C5 1.365(5) . ?
C5 C6 1.425(4) . ?
C6 C7 1.420(4) . ?
C6 C8 1.436(4) . ?
C10 C11 1.378(4) . ?
C10 C15 1.431(4) . ?
C11 C12 1.402(5) . ?
C12 C13 1.371(5) . ?
C13 C14 1.413(4) . ?
C14 C15 1.419(4) . ?
C14 C16 1.455(4) . ?
C18 C19 1.384(4) . ?
C18 C23 1.408(4) . ?
C19 C20 1.386(4) . ?
C20 C21 1.381(4) . ?
C21 C22 1.405(4) . ?
C22 C23 1.396(4) . ?
C22 C24 1.459(4) . ?
C25 C26 1.508(6) . ?
C27 C28 1.534(4) . ?
C29 C30 1.521(4) . ?
O7 C31 1.324(10) . ?
O8 C32 1.411(9) . ?
