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#$Date: 2022-09-03 02:03:18 +0300 (Sat, 03 Sep 2022) $
#$Revision: 277607 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/11/7711129.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_7711129
loop_
_publ_author_name
'Youssef, Heba'
'Schäfer, Thomas C.'
'Becker, Jonathan'
'Sedykh, Alexander E.'
'Basso, Leonardo'
'Pietzonka, Clemens'
'Taydakov, Ilya V.'
'Kraus, Florian'
'Müller-Buschbaum, Klaus'
_publ_section_title
;
 3D-Frameworks and 2D-Networks of Lanthanide Coordination Polymers with
 3-Pyridylpyrazole: Photophysical and Magnetic Properties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01999J
_journal_year                    2022
_chemical_formula_sum            'C8 H8 Cl4 La N3'
_chemical_formula_weight         426.88
_chemical_name_systematic        14
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-08-29 deposited with the CCDC.	2022-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.213(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.480(3)
_cell_length_b                   8.8310(19)
_cell_length_c                   21.086(5)
_cell_measurement_reflns_used    6777
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.87
_cell_measurement_theta_min      2.76
_cell_volume                     2490.3(10)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2015)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.887
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measurement_device_type  'Bruker PHOTON100'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0900
_diffrn_reflns_Laue_measured_fraction_full 0.887
_diffrn_reflns_Laue_measured_fraction_max 0.856
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2396
_diffrn_reflns_point_group_measured_fraction_full 0.887
_diffrn_reflns_point_group_measured_fraction_max 0.856
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.947
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    4.262
_exptl_absorpt_correction_T_max  0.746067
_exptl_absorpt_correction_T_min  0.647713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.037
_exptl_crystal_size_min          0.019
_refine_diff_density_max         1.397
_refine_diff_density_min         -1.395
_refine_diff_density_rms         0.327
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.215
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         2396
_refine_ls_number_restraints     193
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.1145
_refine_ls_R_factor_gt           0.0857
_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)+(0.0260P)²+287.8564P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1576
_refine_ls_wR_factor_ref         0.1669
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1981
_reflns_number_total             2396
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt01999j2.cif
_cod_data_source_block           2D_La3-PyPzH2Cl4
_cod_original_cell_volume        2490.2(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7711129
_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. 
;
_shelx_estimated_absorpt_t_min   0.815
_shelx_estimated_absorpt_t_max   0.923
_exptl_absorpt_special_details
;
Semi-empirical absorption corrections were performed by utilizing
the redundancy of the data to analyse equivalent intensities in
terms of a multipolar spherical harmonic expansion and
compensating for it.
;
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
La1 La 0.31918(7) 0.61307(13) 0.24740(7) 0.0039(3) Uani 1 1 d . . . . .
Cl1 Cl 0.3567(4) 0.9253(5) 0.2387(3) 0.0111(11) Uani 1 1 d . . . . .
Cl2 Cl 0.2330(4) 0.5886(6) 0.1194(2) 0.0130(11) Uani 1 1 d . . . . .
Cl3 Cl 0.3666(3) 0.2986(5) 0.2485(3) 0.0096(10) Uani 1 1 d . . . . .
Cl4 Cl 0.5119(4) 0.6198(6) 0.32998(18) 0.0095(8) Uani 1 1 d . . . . .
N1 N 0.4827(16) 0.811(2) 0.6311(9) 0.0148(16) Uani 1 1 d . U . . .
H1A H 0.510732 0.769114 0.666695 0.018 Uiso 1 1 calc R U . . .
N2 N 0.3259(13) 0.736(2) 0.4138(8) 0.0148(16) Uani 1 1 d . U . . .
H2A H 0.324643 0.831908 0.403106 0.018 Uiso 1 1 calc R U . . .
N3 N 0.2949(14) 0.627(2) 0.3734(9) 0.0148(16) Uani 1 1 d . U . . .
C1 C 0.4452(15) 0.719(3) 0.5814(10) 0.015(3) Uani 1 1 d . U . . .
H1 H 0.449572 0.611997 0.585226 0.018 Uiso 1 1 calc R U . . .
C2 C 0.478(2) 0.962(3) 0.6276(11) 0.018(3) Uani 1 1 d . U . . .
H2 H 0.509232 1.020953 0.662212 0.021 Uiso 1 1 calc R U . . .
C3 C 0.4308(15) 1.031(3) 0.5758(10) 0.014(3) Uani 1 1 d . U . . .
H3 H 0.424427 1.138218 0.574702 0.017 Uiso 1 1 calc R U . . .
C4 C 0.3913(16) 0.945(3) 0.5243(10) 0.0127(16) Uani 1 1 d . U . . .
H4 H 0.357399 0.993388 0.487562 0.015 Uiso 1 1 calc R U . . .
C5 C 0.4008(16) 0.786(3) 0.5255(10) 0.0127(16) Uani 1 1 d . U . . .
C6 C 0.3604(17) 0.686(3) 0.4743(10) 0.0127(16) Uani 1 1 d . U . . .
C7 C 0.3542(18) 0.527(3) 0.4710(11) 0.016(3) Uani 1 1 d . U . . .
H7 H 0.374076 0.456744 0.504183 0.019 Uiso 1 1 calc R U . . .
C8 C 0.3123(17) 0.496(3) 0.4080(11) 0.017(3) Uani 1 1 d . U . . .
H8 H 0.297937 0.397431 0.391549 0.021 Uiso 1 1 calc R U . . .
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 '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
N3 La1 Cl2 148.8(4) . . ?
N3 La1 Cl1 93.6(5) . . ?
Cl2 La1 Cl1 93.94(17) . . ?
N3 La1 Cl3 95.3(5) . . ?
Cl2 La1 Cl3 89.90(17) . . ?
Cl1 La1 Cl3 156.04(12) . . ?
N3 La1 Cl1 74.4(4) . 4_545 ?
Cl2 La1 Cl1 79.10(16) . 4_545 ?
Cl1 La1 Cl1 135.52(11) . 4_545 ?
Cl3 La1 Cl1 68.41(13) . 4_545 ?
N3 La1 Cl4 68.1(4) . . ?
Cl2 La1 Cl4 142.99(15) . . ?
Cl1 La1 Cl4 82.33(15) . . ?
Cl3 La1 Cl4 80.45(15) . . ?
Cl1 La1 Cl4 128.03(15) 4_545 . ?
N3 La1 Cl4 137.0(4) . 2_655 ?
Cl2 La1 Cl4 74.13(14) . 2_655 ?
Cl1 La1 Cl4 77.74(15) . 2_655 ?
Cl3 La1 Cl4 80.62(15) . 2_655 ?
Cl1 La1 Cl4 138.75(15) 4_545 2_655 ?
Cl4 La1 Cl4 69.08(12) . 2_655 ?
N3 La1 Cl3 75.1(4) . 4 ?
Cl2 La1 Cl3 79.83(16) . 4 ?
Cl1 La1 Cl3 67.94(12) . 4 ?
Cl3 La1 Cl3 135.94(11) . 4 ?
Cl1 La1 Cl3 67.59(11) 4_545 4 ?
Cl4 La1 Cl3 130.54(15) . 4 ?
Cl4 La1 Cl3 134.90(15) 2_655 4 ?
La1 Cl1 La1 113.12(16) . 4 ?
La1 Cl3 La1 110.19(14) . 4_545 ?
La1 Cl4 La1 110.87(12) . 2_655 ?
C2 N1 C1 123(2) . . ?
N3 N2 C6 114.3(19) . . ?
N2 N3 C8 104.4(17) . . ?
N2 N3 La1 126.9(14) . . ?
C8 N3 La1 116.5(15) . . ?
N1 C1 C5 118(2) . . ?
N1 C2 C3 121(2) . . ?
C2 C3 C4 119(2) . . ?
C3 C4 C5 121(2) . . ?
C1 C5 C4 118(2) . . ?
C1 C5 C6 117(2) . . ?
C4 C5 C6 125(2) . . ?
N2 C6 C7 105(2) . . ?
N2 C6 C5 123(2) . . ?
C7 C6 C5 131(2) . . ?
C6 C7 C8 105(2) . . ?
N3 C8 C7 111(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
La1 N3 2.720(18) . ?
La1 Cl2 2.809(5) . ?
La1 Cl1 2.814(5) . ?
La1 Cl3 2.849(5) . ?
La1 Cl1 2.938(5) 4_545 ?
La1 Cl4 2.941(5) . ?
La1 Cl4 2.964(5) 2_655 ?
La1 Cl3 3.003(5) 4 ?
N1 C2 1.33(2) . ?
N1 C1 1.37(3) . ?
N2 N3 1.31(3) . ?
N2 C6 1.37(3) . ?
N3 C8 1.37(3) . ?
C1 C5 1.38(3) . ?
C2 C3 1.34(3) . ?
C3 C4 1.38(3) . ?
C4 C5 1.42(3) . ?
C5 C6 1.45(3) . ?
C6 C7 1.40(3) . ?
C7 C8 1.40(3) . ?
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
N1 H1A Cl3 0.88 2.35 3.20(2) 160.2 5_666 yes
N1 H1A Cl3 0.88 2.82 3.24(2) 110.9 6_566 yes
N2 H2A Cl2 0.88 2.42 3.27(2) 161.8 4 yes
