#------------------------------------------------------------------------------
#$Date: 2021-11-06 20:55:40 +0100 (Sat 06 de Nov de 2021) $
#$Revision: 270438 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/35/7243586.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_7243586
loop_
_publ_author_name
'Dailey, Maegan'
'Besson, Claire'
_publ_section_title
;
 Selective crystallization of four bis(phthalocyaninato)lanthanoid(iii)
 polymorphs
;
_journal_issue                   40
_journal_name_full               CrystEngComm
_journal_page_first              7151
_journal_page_last               7161
_journal_paper_doi               10.1039/D1CE00936B
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C64 H32 N16 Tb'
_chemical_formula_sum            'C64 H32 N16 Tb'
_chemical_formula_weight         1183.97
_chemical_name_common            bis(phthalocyaninato)-terbium
_chemical_name_systematic
(phthalocyaninato)-(phthalocyaninato-radical)-terbium(III)
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-09-09 deposited with the CCDC.	2021-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.708(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.086(3)
_cell_length_b                   14.160(2)
_cell_length_c                   13.1416(14)
_cell_measurement_reflns_used    42659
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      55.447
_cell_measurement_theta_min      5.243
_cell_volume                     4709.1(11)
_computing_cell_refinement       'APEX3 v2019.1-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service V6.2.132'
_computing_data_reduction        'SAINT V8.40A (Bruker Nanon Inc., 2019)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle rev 958)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1427
_diffrn_reflns_av_unetI/netI     0.0742
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            41290
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.962
_diffrn_reflns_theta_min         2.115
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    1.569
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (G. Sheldrick)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             2372
_exptl_crystal_size_max          0.541
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.701
_refine_diff_density_min         -1.201
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         5651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0373P)²+6.6728P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.0996
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4699
_reflns_number_total             5651
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ce00936b2.cif
_cod_data_source_block           TbPc2_C2c
_cod_depositor_comments
'Adding full bibliography for 7243585--7243607.cif.'
_cod_original_cell_volume        4708.9(11)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7243586
_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.
;
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
Tb01 Tb 0.500000 0.59160(2) 0.250000 0.01527(8) Uani 1 2 d S T P . .
N1 N 0.38510(14) 0.5059(3) 0.2910(3) 0.0200(8) Uani 1 1 d . . . . .
C1 C 0.42493(17) 0.4451(3) 0.3163(3) 0.0206(9) Uani 1 1 d . . . . .
N2 N 0.47650(13) 0.4652(3) 0.3443(3) 0.0186(7) Uani 1 1 d . . . . .
C2 C 0.41718(16) 0.3431(3) 0.3157(4) 0.0203(9) Uani 1 1 d . . . . .
N3 N 0.55597(13) 0.3693(2) 0.4085(3) 0.0186(7) Uani 1 1 d . . . . .
C3 C 0.37207(17) 0.2877(3) 0.2813(4) 0.0233(9) Uani 1 1 d . . . . .
H3 H 0.338315 0.315364 0.260699 0.028 Uiso 1 1 calc R U . . .
C4 C 0.37799(19) 0.1898(3) 0.2778(4) 0.0283(10) Uani 1 1 d . . . . .
H4 H 0.347718 0.150277 0.253069 0.034 Uiso 1 1 calc R U . . .
N4 N 0.57779(13) 0.5364(3) 0.4118(3) 0.0192(7) Uani 1 1 d . . . . .
C5 C 0.42783(19) 0.1496(3) 0.3104(4) 0.0293(11) Uani 1 1 d . . . . .
H5 H 0.430932 0.082996 0.307464 0.035 Uiso 1 1 calc R U . . .
N5 N 0.63095(13) 0.6786(3) 0.4571(3) 0.0193(7) Uani 1 1 d . . . . .
N6 N 0.53800(13) 0.7200(2) 0.3818(3) 0.0177(7) Uani 1 1 d . . . . .
C6 C 0.47310(17) 0.2053(3) 0.3470(4) 0.0239(9) Uani 1 1 d . . . . .
H6 H 0.507000 0.177589 0.369833 0.029 Uiso 1 1 calc R U . . .
C7 C 0.46721(16) 0.3017(3) 0.3491(4) 0.0208(9) Uani 1 1 d . . . . .
N7 N 0.46003(14) 0.8141(3) 0.3457(3) 0.0198(7) Uani 1 1 d . . . . .
N8 N 0.43689(14) 0.6478(2) 0.3165(3) 0.0189(7) Uani 1 1 d . . . . .
C8 C 0.50380(17) 0.3816(3) 0.3705(4) 0.0210(9) Uani 1 1 d . . . . .
C9 C 0.58954(17) 0.4415(3) 0.4287(3) 0.0202(9) Uani 1 1 d . . . . .
C10 C 0.64701(16) 0.4295(3) 0.4749(3) 0.0203(9) Uani 1 1 d . . . . .
C11 C 0.67867(17) 0.3499(3) 0.5011(4) 0.0238(9) Uani 1 1 d . . . . .
H11 H 0.664144 0.288158 0.491695 0.029 Uiso 1 1 calc R U . . .
C12 C 0.73321(18) 0.3648(3) 0.5422(4) 0.0280(10) Uani 1 1 d . . . . .
H12 H 0.756193 0.311759 0.561398 0.034 Uiso 1 1 calc R U . . .
C14 C 0.72242(17) 0.5337(3) 0.5285(4) 0.0247(10) Uani 1 1 d . . . . .
H14 H 0.736985 0.595399 0.537345 0.030 Uiso 1 1 calc R U . . .
C15 C 0.66843(17) 0.5197(3) 0.4881(4) 0.0222(9) Uani 1 1 d . . . . .
C16 C 0.62419(15) 0.5848(3) 0.4508(3) 0.0186(8) Uani 1 1 d . . . . .
C17 C 0.59106(17) 0.7400(3) 0.4284(3) 0.0191(9) Uani 1 1 d . . . . .
C18 C 0.59939(16) 0.8412(3) 0.4499(4) 0.0205(9) Uani 1 1 d . . . . .
C19 C 0.64481(17) 0.8960(3) 0.4954(4) 0.0258(10) Uani 1 1 d . . . . .
H19 H 0.678805 0.869427 0.516038 0.031 Uiso 1 1 calc R U . . .
C20 C 0.63828(18) 0.9917(3) 0.5095(4) 0.0292(10) Uani 1 1 d . . . . .
H20 H 0.668568 1.031223 0.541418 0.035 Uiso 1 1 calc R U . . .
C21 C 0.58833(18) 1.0312(3) 0.4779(4) 0.0296(11) Uani 1 1 d . . . . .
H21 H 0.585354 1.096889 0.488805 0.036 Uiso 1 1 calc R U . . .
C22 C 0.54308(18) 0.9766(3) 0.4312(4) 0.0245(9) Uani 1 1 d . . . . .
H22 H 0.509018 1.003469 0.409016 0.029 Uiso 1 1 calc R U . . .
C23 C 0.54959(17) 0.8811(3) 0.4180(4) 0.0212(9) Uani 1 1 d . . . . .
C24 C 0.51176(17) 0.8022(3) 0.3774(3) 0.0207(9) Uani 1 1 d . . . . .
C25 C 0.42633(16) 0.7418(3) 0.3199(3) 0.0194(9) Uani 1 1 d . . . . .
C26 C 0.37015(16) 0.7548(3) 0.2913(4) 0.0212(9) Uani 1 1 d . . . . .
C27 C 0.33936(18) 0.8349(3) 0.2794(4) 0.0262(10) Uani 1 1 d . . . . .
H27 H 0.354493 0.896257 0.293519 0.031 Uiso 1 1 calc R U . . .
C28 C 0.28558(17) 0.8214(3) 0.2459(4) 0.0270(10) Uani 1 1 d . . . . .
H28 H 0.263604 0.874411 0.238457 0.032 Uiso 1 1 calc R U . . .
C29 C 0.26351(17) 0.7317(4) 0.2233(4) 0.0280(10) Uani 1 1 d . . . . .
H29 H 0.226487 0.724859 0.198359 0.034 Uiso 1 1 calc R U . . .
C30 C 0.29439(17) 0.6513(3) 0.2363(4) 0.0250(10) Uani 1 1 d . . . . .
H30 H 0.279296 0.589884 0.221247 0.030 Uiso 1 1 calc R U . . .
C31 C 0.34807(16) 0.6653(3) 0.2721(3) 0.0213(9) Uani 1 1 d . . . . .
C32 C 0.39116(16) 0.5989(3) 0.2927(3) 0.0192(8) Uani 1 1 d . . . . .
C13 C 0.75434(18) 0.4541(3) 0.5553(4) 0.0286(10) Uani 1 1 d . . . . .
H13 H 0.791512 0.461435 0.583413 0.034 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'
Tb Tb -0.1723 4.1537 '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
N6 Tb01 N6 82.44(16) 2_655 . ?
N6 Tb01 N4 70.36(12) 2_655 2_655 ?
N6 Tb01 N4 145.19(12) . 2_655 ?
N6 Tb01 N4 145.19(12) 2_655 . ?
N6 Tb01 N4 70.36(12) . . ?
N4 Tb01 N4 142.39(17) 2_655 . ?
N6 Tb01 N8 70.09(12) 2_655 2_655 ?
N6 Tb01 N8 81.21(11) . 2_655 ?
N4 Tb01 N8 108.12(11) 2_655 2_655 ?
N4 Tb01 N8 84.28(12) . 2_655 ?
N6 Tb01 N8 81.21(11) 2_655 . ?
N6 Tb01 N8 70.09(12) . . ?
N4 Tb01 N8 84.29(12) 2_655 . ?
N4 Tb01 N8 108.12(11) . . ?
N8 Tb01 N8 141.70(17) 2_655 . ?
N6 Tb01 N2 108.80(11) 2_655 2_655 ?
N6 Tb01 N2 141.98(11) . 2_655 ?
N4 Tb01 N2 69.84(12) 2_655 2_655 ?
N4 Tb01 N2 82.46(12) . 2_655 ?
N8 Tb01 N2 69.80(12) 2_655 2_655 ?
N8 Tb01 N2 146.04(12) . 2_655 ?
N6 Tb01 N2 141.98(11) 2_655 . ?
N6 Tb01 N2 108.80(11) . . ?
N4 Tb01 N2 82.46(12) 2_655 . ?
N4 Tb01 N2 69.85(12) . . ?
N8 Tb01 N2 146.04(12) 2_655 . ?
N8 Tb01 N2 69.80(12) . . ?
N2 Tb01 N2 84.88(16) 2_655 . ?
C32 N1 C1 123.3(4) . . ?
N1 C1 N2 127.7(4) . . ?
N1 C1 C2 122.0(4) . . ?
N2 C1 C2 110.3(4) . . ?
C1 N2 C8 107.6(4) . . ?
C1 N2 Tb01 120.6(3) . . ?
C8 N2 Tb01 121.3(3) . . ?
C3 C2 C7 120.9(4) . . ?
C3 C2 C1 132.3(4) . . ?
C7 C2 C1 106.6(4) . . ?
C9 N3 C8 122.6(4) . . ?
C2 C3 C4 117.8(4) . . ?
C2 C3 H3 121.1 . . ?
C4 C3 H3 121.1 . . ?
C5 C4 C3 120.8(4) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C16 N4 C9 107.9(3) . . ?
C16 N4 Tb01 121.3(3) . . ?
C9 N4 Tb01 121.1(3) . . ?
C6 C5 C4 121.3(4) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
C17 N5 C16 123.3(4) . . ?
C24 N6 C17 107.7(4) . . ?
C24 N6 Tb01 123.2(3) . . ?
C17 N6 Tb01 122.1(3) . . ?
C7 C6 C5 117.9(4) . . ?
C7 C6 H6 121.0 . . ?
C5 C6 H6 121.0 . . ?
C6 C7 C2 121.3(4) . . ?
C6 C7 C8 133.3(4) . . ?
C2 C7 C8 105.0(4) . . ?
C25 N7 C24 122.5(4) . . ?
C25 N8 C32 107.7(3) . . ?
C25 N8 Tb01 122.2(3) . . ?
C32 N8 Tb01 120.7(3) . . ?
N3 C8 N2 127.4(4) . . ?
N3 C8 C7 122.2(4) . . ?
N2 C8 C7 110.3(4) . . ?
N3 C9 N4 127.9(4) . . ?
N3 C9 C10 123.2(4) . . ?
N4 C9 C10 108.9(4) . . ?
C11 C10 C15 121.4(4) . . ?
C11 C10 C9 132.1(4) . . ?
C15 C10 C9 106.5(4) . . ?
C10 C11 C12 116.8(4) . . ?
C10 C11 H11 121.6 . . ?
C12 C11 H11 121.6 . . ?
C13 C12 C11 121.7(4) . . ?
C13 C12 H12 119.1 . . ?
C11 C12 H12 119.1 . . ?
C15 C14 C13 117.4(4) . . ?
C15 C14 H14 121.3 . . ?
C13 C14 H14 121.3 . . ?
C14 C15 C10 121.4(4) . . ?
C14 C15 C16 132.3(4) . . ?
C10 C15 C16 106.3(4) . . ?
N5 C16 N4 127.6(4) . . ?
N5 C16 C15 122.1(4) . . ?
N4 C16 C15 110.3(4) . . ?
N5 C17 N6 127.3(4) . . ?
N5 C17 C18 122.7(4) . . ?
N6 C17 C18 109.9(4) . . ?
C19 C18 C23 121.2(4) . . ?
C19 C18 C17 132.3(4) . . ?
C23 C18 C17 106.5(4) . . ?
C18 C19 C20 116.9(4) . . ?
C18 C19 H19 121.5 . . ?
C20 C19 H19 121.5 . . ?
C19 C20 C21 121.6(4) . . ?
C19 C20 H20 119.2 . . ?
C21 C20 H20 119.2 . . ?
C22 C21 C20 121.3(4) . . ?
C22 C21 H21 119.3 . . ?
C20 C21 H21 119.3 . . ?
C21 C22 C23 117.1(4) . . ?
C21 C22 H22 121.5 . . ?
C23 C22 H22 121.5 . . ?
C22 C23 C18 121.8(4) . . ?
C22 C23 C24 132.2(4) . . ?
C18 C23 C24 105.9(4) . . ?
N7 C24 N6 127.9(4) . . ?
N7 C24 C23 122.2(4) . . ?
N6 C24 C23 109.9(4) . . ?
N7 C25 N8 127.9(4) . . ?
N7 C25 C26 122.3(4) . . ?
N8 C25 C26 109.7(4) . . ?
C31 C26 C27 121.1(4) . . ?
C31 C26 C25 106.2(4) . . ?
C27 C26 C25 132.6(4) . . ?
C28 C27 C26 117.4(4) . . ?
C28 C27 H27 121.3 . . ?
C26 C27 H27 121.3 . . ?
C29 C28 C27 121.1(4) . . ?
C29 C28 H28 119.5 . . ?
C27 C28 H28 119.5 . . ?
C28 C29 C30 121.6(4) . . ?
C28 C29 H29 119.2 . . ?
C30 C29 H29 119.2 . . ?
C31 C30 C29 116.9(4) . . ?
C31 C30 H30 121.6 . . ?
C29 C30 H30 121.6 . . ?
C26 C31 C30 121.9(4) . . ?
C26 C31 C32 106.6(4) . . ?
C30 C31 C32 131.5(4) . . ?
N1 C32 N8 127.3(4) . . ?
N1 C32 C31 123.0(4) . . ?
N8 C32 C31 109.6(4) . . ?
C12 C13 C14 121.3(4) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
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
Tb01 N6 2.417(3) 2_655 ?
Tb01 N6 2.417(3) . ?
Tb01 N4 2.424(3) 2_655 ?
Tb01 N4 2.424(3) . ?
Tb01 N8 2.425(3) 2_655 ?
Tb01 N8 2.425(3) . ?
Tb01 N2 2.426(3) 2_655 ?
Tb01 N2 2.426(3) . ?
N1 C32 1.327(5) . ?
N1 C1 1.334(5) . ?
C1 N2 1.361(5) . ?
C1 C2 1.460(6) . ?
N2 C8 1.371(5) . ?
C2 C3 1.389(6) . ?
C2 C7 1.406(6) . ?
N3 C9 1.336(5) . ?
N3 C8 1.338(5) . ?
C3 C4 1.399(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.395(6) . ?
C4 H4 0.9500 . ?
N4 C16 1.360(5) . ?
N4 C9 1.379(5) . ?
C5 C6 1.392(6) . ?
C5 H5 0.9500 . ?
N5 C17 1.337(5) . ?
N5 C16 1.340(5) . ?
N6 C24 1.365(5) . ?
N6 C17 1.373(5) . ?
C6 C7 1.377(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.471(6) . ?
N7 C25 1.334(5) . ?
N7 C24 1.337(5) . ?
N8 C25 1.369(5) . ?
N8 C32 1.370(5) . ?
C9 C10 1.467(6) . ?
C10 C11 1.383(6) . ?
C10 C15 1.391(6) . ?
C11 C12 1.402(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.376(7) . ?
C12 H12 0.9500 . ?
C14 C15 1.387(6) . ?
C14 C13 1.387(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.451(6) . ?
C17 C18 1.459(6) . ?
C18 C19 1.388(6) . ?
C18 C23 1.394(6) . ?
C19 C20 1.390(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.396(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.383(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.386(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.473(6) . ?
C25 C26 1.466(6) . ?
C26 C31 1.385(6) . ?
C26 C27 1.393(6) . ?
C27 C28 1.391(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.387(7) . ?
C28 H28 0.9500 . ?
C29 C30 1.396(6) . ?
C29 H29 0.9500 . ?
C30 C31 1.385(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.462(6) . ?
C13 H13 0.9500 . ?
