#------------------------------------------------------------------------------
#$Date: 2021-02-03 21:55:52 +0200 (Wed, 03 Feb 2021) $
#$Revision: 261398 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/84/4518452.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_4518452
loop_
_publ_author_name
'Lu, Huangjie'
'Zheng, Zhaofa'
'Li, Zi-Jian'
'Bao, Hongliang'
'Guo, Xiaojing'
'Guo, Xiaofeng'
'Lin, Jian'
'Qian, Yuan'
'Wang, Jian-Qiang'
_publ_section_title
;
 Achieving UV and X-ray Dual Photochromism in a Metal-Organic Hybrid via
 Structural Modulation.
;
_journal_issue                   2
_journal_name_full               'ACS applied materials & interfaces'
_journal_page_first              2745
_journal_page_last               2752
_journal_paper_doi               10.1021/acsami.0c20036
_journal_volume                  13
_journal_year                    2021
_chemical_formula_moiety         'C18 N3 O6 Tm'
_chemical_formula_sum            'C18 N3 O6 Tm'
_chemical_formula_weight         523.14
_chemical_melting_point          ?
_chemical_name_common
'Thulium 2,2':6',2''-terpyridine-4'-carboxyli'
_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'
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 125.1750(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9101(7)
_cell_length_b                   9.4336(3)
_cell_length_c                   11.8747(4)
_cell_measurement_reflns_used    9550
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      55.056
_cell_measurement_theta_min      5.136
_cell_volume                     1639.95(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '0.5 wide w/ exposures'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11425
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.528
_diffrn_reflns_theta_min         2.568
_exptl_absorpt_coefficient_mu    5.454
_exptl_absorpt_correction_T_max  0.580
_exptl_absorpt_correction_T_min  0.416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SHELTXPREP
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.119
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1880
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0187
_refine_ls_R_factor_gt           0.0183
_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)+(0.0362P)²+3.8735P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0543
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1853
_reflns_number_total             1880
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            am0c20036_si_002.cif
_cod_data_source_block           TmTPC-2beforeXray
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'N/a' was changed to '?' --
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4518452
_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.
;
_shelxl_version_number           2014-3
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
Tm1 Tm 0.5000 -0.16000(2) 0.7500 0.01908(8) Uani 1 2 d S T P . .
N1 N 0.5000 0.5773(4) 0.7500 0.0175(6) Uani 1 2 d S T P . .
N2 N 0.58985(17) 0.7344(3) 0.6778(3) 0.0232(5) Uani 1 1 d . . . . .
O1 O 0.48383(18) 0.0608(2) 0.8268(3) 0.0324(5) Uani 1 1 d . . . . .
O2 O 0.39708(19) -0.2272(3) 0.5143(3) 0.0462(7) Uani 1 1 d . . . . .
O3 O 0.3381(2) -0.0794(3) 0.5827(3) 0.0492(7) Uani 1 1 d . . . . .
C1 C 0.54529(18) 0.5051(3) 0.7091(3) 0.0196(5) Uani 1 1 d . . . . .
C2 C 0.5000 0.1249(5) 0.7500 0.0275(9) Uani 1 2 d S T P . .
C3 C 0.5000 0.2847(4) 0.7500 0.0215(8) Uani 1 2 d S T P . .
C4 C 0.59579(19) 0.5929(3) 0.6692(3) 0.0201(5) Uani 1 1 d . . . . .
C5 C 0.5447(2) 0.3579(3) 0.7036(3) 0.0225(6) Uani 1 1 d . . . . .
C6 C 0.3350(3) -0.1561(3) 0.4948(4) 0.0334(8) Uani 1 1 d . . . . .
C7 C 0.6341(3) 0.8196(3) 0.6430(4) 0.0309(7) Uani 1 1 d . . . . .
C8 C 0.6474(2) 0.5334(3) 0.6285(3) 0.0278(6) Uani 1 1 d . . . . .
C9 C 0.6950(3) 0.6213(4) 0.5962(4) 0.0338(7) Uani 1 1 d . . . . .
C10 C 0.6873(2) 0.7673(4) 0.6021(4) 0.0340(7) 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'
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'
Tm Tm -0.3139 5.2483 '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 Tm1 O1 55.89(11) 2_656 . ?
O1 Tm1 O2 87.99(10) 2_656 . ?
O1 Tm1 O2 120.31(9) . . ?
O1 Tm1 O2 120.30(9) 2_656 2_656 ?
O1 Tm1 O2 87.98(10) . 2_656 ?
O2 Tm1 O2 149.18(14) . 2_656 ?
O1 Tm1 N2 138.81(8) 2_656 2_646 ?
O1 Tm1 N2 88.38(8) . 2_646 ?
O2 Tm1 N2 94.81(10) . 2_646 ?
O2 Tm1 N2 72.44(9) 2_656 2_646 ?
O1 Tm1 N2 88.38(8) 2_656 1_545 ?
O1 Tm1 N2 138.81(8) . 1_545 ?
O2 Tm1 N2 72.44(9) . 1_545 ?
O2 Tm1 N2 94.81(10) 2_656 1_545 ?
N2 Tm1 N2 131.60(12) 2_646 1_545 ?
O1 Tm1 N1 152.06(5) 2_656 1_545 ?
O1 Tm1 N1 152.05(5) . 1_545 ?
O2 Tm1 N1 74.59(7) . 1_545 ?
O2 Tm1 N1 74.59(7) 2_656 1_545 ?
N2 Tm1 N1 65.80(6) 2_646 1_545 ?
N2 Tm1 N1 65.80(6) 1_545 1_545 ?
O1 Tm1 O3 76.67(10) 2_656 . ?
O1 Tm1 O3 72.26(10) . . ?
O2 Tm1 O3 52.54(10) . . ?
O2 Tm1 O3 140.28(10) 2_656 . ?
N2 Tm1 O3 72.88(10) 2_646 . ?
N2 Tm1 O3 122.87(9) 1_545 . ?
N1 Tm1 O3 107.63(8) 1_545 . ?
O1 Tm1 O3 72.26(10) 2_656 2_656 ?
O1 Tm1 O3 76.68(10) . 2_656 ?
O2 Tm1 O3 140.28(10) . 2_656 ?
O2 Tm1 O3 52.54(10) 2_656 2_656 ?
N2 Tm1 O3 122.87(9) 2_646 2_656 ?
N2 Tm1 O3 72.88(10) 1_545 2_656 ?
N1 Tm1 O3 107.63(8) 1_545 2_656 ?
O3 Tm1 O3 144.74(15) . 2_656 ?
O1 Tm1 C2 27.94(5) 2_656 . ?
O1 Tm1 C2 27.95(5) . . ?
O2 Tm1 C2 105.41(7) . . ?
O2 Tm1 C2 105.41(7) 2_656 . ?
N2 Tm1 C2 114.20(6) 2_646 . ?
N2 Tm1 C2 114.20(6) 1_545 . ?
N1 Tm1 C2 180.0 1_545 . ?
O3 Tm1 C2 72.37(8) . . ?
O3 Tm1 C2 72.37(8) 2_656 . ?
O1 Tm1 C6 81.72(9) 2_656 . ?
O1 Tm1 C6 96.93(9) . . ?
O2 Tm1 C6 25.74(10) . . ?
O2 Tm1 C6 155.20(11) 2_656 . ?
N2 Tm1 C6 83.38(10) 2_646 . ?
N2 Tm1 C6 97.25(10) 1_545 . ?
N1 Tm1 C6 90.76(6) 1_545 . ?
O3 Tm1 C6 26.80(10) . . ?
O3 Tm1 C6 152.20(10) 2_656 . ?
C2 Tm1 C6 89.24(6) . . ?
O1 Tm1 C6 96.93(10) 2_656 2_656 ?
O1 Tm1 C6 81.72(10) . 2_656 ?
O2 Tm1 C6 155.20(11) . 2_656 ?
O2 Tm1 C6 25.74(10) 2_656 2_656 ?
N2 Tm1 C6 97.25(10) 2_646 2_656 ?
N2 Tm1 C6 83.38(10) 1_545 2_656 ?
N1 Tm1 C6 90.76(6) 1_545 2_656 ?
O3 Tm1 C6 152.20(10) . 2_656 ?
O3 Tm1 C6 26.80(10) 2_656 2_656 ?
C2 Tm1 C6 89.24(6) . 2_656 ?
C6 Tm1 C6 178.49(13) . 2_656 ?
C1 N1 C1 119.2(3) . 2_656 ?
C1 N1 Tm1 120.41(17) . 1_565 ?
C1 N1 Tm1 120.41(17) 2_656 1_565 ?
C4 N2 C7 118.7(3) . . ?
C4 N2 Tm1 122.01(18) . 1_565 ?
C7 N2 Tm1 119.3(2) . 1_565 ?
C2 O1 Tm1 90.7(2) . . ?
C6 O2 Tm1 94.7(2) . . ?
C6 O3 Tm1 87.8(2) . . ?
N1 C1 C5 122.2(3) . . ?
N1 C1 C4 115.8(2) . . ?
C5 C1 C4 122.0(3) . . ?
O1 C2 O1 122.6(4) 2_656 . ?
O1 C2 C3 118.7(2) 2_656 . ?
O1 C2 C3 118.7(2) . . ?
O1 C2 Tm1 61.3(2) 2_656 . ?
O1 C2 Tm1 61.3(2) . . ?
C3 C2 Tm1 180.0 . . ?
C5 C3 C5 120.4(4) . 2_656 ?
C5 C3 C2 119.79(19) . . ?
C5 C3 C2 119.79(19) 2_656 . ?
N2 C4 C8 121.7(3) . . ?
N2 C4 C1 115.9(2) . . ?
C8 C4 C1 122.3(3) . . ?
C3 C5 C1 117.9(3) . . ?
O2 C6 O3 125.0(4) . . ?
O2 C6 Tm1 59.6(2) . . ?
O3 C6 Tm1 65.4(2) . . ?
N2 C7 C10 122.6(3) . . ?
C4 C8 C9 119.5(3) . . ?
C10 C9 C8 118.9(3) . . ?
C7 C10 C9 118.6(3) . . ?
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
Tm1 O1 2.358(2) 2_656 ?
Tm1 O1 2.358(2) . ?
Tm1 O2 2.385(3) . ?
Tm1 O2 2.385(3) 2_656 ?
Tm1 N2 2.431(2) 2_646 ?
Tm1 N2 2.431(2) 1_545 ?
Tm1 N1 2.478(3) 1_545 ?
Tm1 O3 2.509(3) . ?
Tm1 O3 2.509(3) 2_656 ?
Tm1 C2 2.687(5) . ?
Tm1 C6 2.757(4) . ?
Tm1 C6 2.757(4) 2_656 ?
N1 C1 1.346(3) . ?
N1 C1 1.346(3) 2_656 ?
N1 Tm1 2.478(3) 1_565 ?
N2 C4 1.347(4) . ?
N2 C7 1.351(4) . ?
N2 Tm1 2.431(2) 1_565 ?
O1 C2 1.260(3) . ?
O2 C6 1.201(5) . ?
O3 C6 1.244(5) . ?
C1 C5 1.390(4) . ?
C1 C4 1.491(4) . ?
C2 O1 1.259(3) 2_656 ?
C2 C3 1.508(6) . ?
C3 C5 1.390(4) . ?
C3 C5 1.390(4) 2_656 ?
C4 C8 1.385(4) . ?
C7 C10 1.385(5) . ?
C8 C9 1.392(5) . ?
C9 C10 1.390(5) . ?
