#------------------------------------------------------------------------------
#$Date: 2019-11-26 05:26:48 +0200 (Tue, 26 Nov 2019) $
#$Revision: 242710 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/28/4132809.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_4132809
loop_
_publ_author_name
'Yamabayashi, Tsutomu'
'Atzori, Matteo'
'Tesi, Lorenzo'
'Cosquer, Goulven'
'Santanni, Fabio'
'Boulon, Marie-Emmanuelle'
'Morra, Elena'
'Benci, Stefano'
'Torre, Renato'
'Chiesa, Mario'
'Sorace, Lorenzo'
'Sessoli, Roberta'
'Yamashita, Masahiro'
_publ_section_title
;
 Scaling Up Electronic Spin Qubits into a Three-Dimensional Metal-Organic
 Framework.
;
_journal_issue                   38
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12090
_journal_page_last               12101
_journal_paper_doi               10.1021/jacs.8b06733
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C44 H28 N4 O Ti'
_chemical_formula_sum            'C44 H28 N4 O Ti'
_chemical_formula_weight         676.60
_chemical_name_common            'Titanyl Tetraphenylporphyrin'
_space_group_crystal_system      tetragonal
_space_group_IT_number           79
_space_group_name_Hall           'I 4'
_space_group_name_H-M_alt        'I 4'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3796(2)
_cell_length_b                   13.3796(2)
_cell_length_c                   9.7766(3)
_cell_measurement_reflns_used    2905
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.9630
_cell_measurement_theta_min      5.5630
_cell_volume                     1750.15(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.1241
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Xcalibur, Onyx'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4781
_diffrn_reflns_point_group_measured_fraction_full 0.836
_diffrn_reflns_point_group_measured_fraction_max 0.814
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.509
_diffrn_reflns_theta_min         5.605
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.385
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red-violet
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.448
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.222
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.05(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         1424
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0503
_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)+(0.0944P)²+0.1270P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1399
_reflns_Friedel_coverage         0.563
_reflns_Friedel_fraction_full    0.656
_reflns_Friedel_fraction_max     0.626
_reflns_number_gt                1223
_reflns_number_total             1424
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja8b06733_si_003.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4132809
_shelx_shelxl_version_number     2017/1
_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   0.382
_shelx_estimated_absorpt_t_max   0.917
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+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
Ti Ti 0.500000 0.500000 0.4373(2) 0.0348(17) Uani 0.469(10) 4 d S T P A 1
O1 O 0.500000 0.500000 0.2762(15) 0.043(4) Uani 0.469(10) 4 d S T P A 1
Ti' Ti 0.500000 0.500000 0.5535(2) 0.0382(15) Uani 0.531(10) 4 d S T P A 2
O1' O 0.500000 0.500000 0.7202(18) 0.060(4) Uani 0.531(10) 4 d S T P A 2
C1 C 0.63134(16) 0.68665(16) 0.4968(8) 0.0413(6) Uani 1 1 d . . . . .
C2 C 0.62506(18) 0.79380(16) 0.4966(9) 0.0495(7) Uani 1 1 d . . . . .
H2 H 0.678542 0.838198 0.497211 0.059 Uiso 1 1 calc R U . . .
C3 C 0.52720(19) 0.81812(17) 0.4954(10) 0.0510(7) Uani 1 1 d . . . . .
H3 H 0.500719 0.882377 0.493648 0.061 Uiso 1 1 calc R U . . .
C4 C 0.47159(16) 0.72645(16) 0.4973(8) 0.0419(6) Uani 1 1 d . . . . .
C5 C 0.36734(16) 0.72086(16) 0.4949(6) 0.0413(6) Uani 1 1 d . . . . .
C6 C 0.31001(16) 0.81625(17) 0.4968(8) 0.0429(6) Uani 1 1 d . . . . .
C7 C 0.2826(5) 0.8617(5) 0.3733(6) 0.0655(16) Uani 1 1 d . . . . .
H7 H 0.301554 0.833269 0.290427 0.079 Uiso 1 1 calc R U . . .
C8 C 0.2278(6) 0.9485(5) 0.3749(9) 0.0749(18) Uani 1 1 d . . . . .
H8 H 0.209047 0.978405 0.292986 0.090 Uiso 1 1 calc R U . . .
C9 C 0.2001(2) 0.9919(2) 0.4991(13) 0.0677(10) Uani 1 1 d . . . . .
H9 H 0.163421 1.050920 0.500370 0.081 Uiso 1 1 calc R U . . .
C10 C 0.2265(6) 0.9482(5) 0.6152(9) 0.080(2) Uani 1 1 d . . . . .
H10 H 0.207383 0.976122 0.698314 0.096 Uiso 1 1 calc R U . . .
C11 C 0.2830(5) 0.8605(5) 0.6135(7) 0.0692(17) Uani 1 1 d . . . . .
H11 H 0.302369 0.832019 0.696152 0.083 Uiso 1 1 calc R U . . .
N1 N 0.53663(13) 0.64708(13) 0.4963(6) 0.0394(5) 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 '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
O1 Ti N1 105.89(18) . 4_565
O1 Ti N1 105.89(18) . 2_665
N1 Ti N1 85.70(10) 4_565 2_665
O1 Ti N1 105.89(18) . 3_655
N1 Ti N1 148.2(4) 4_565 3_655
N1 Ti N1 85.70(10) 2_665 3_655
O1 Ti N1 105.89(18) . .
N1 Ti N1 85.70(10) 4_565 .
N1 Ti N1 148.2(4) 2_665 .
N1 Ti N1 85.70(10) 3_655 .
O1' Ti' N1 105.41(18) . 2_665
O1' Ti' N1 105.41(18) . 3_655
N1 Ti' N1 85.95(9) 2_665 3_655
O1' Ti' N1 105.41(18) . 4_565
N1 Ti' N1 85.95(9) 2_665 4_565
N1 Ti' N1 149.2(4) 3_655 4_565
O1' Ti' N1 105.41(18) . .
N1 Ti' N1 149.2(4) 2_665 .
N1 Ti' N1 85.95(9) 3_655 .
N1 Ti' N1 85.95(9) 4_565 .
N1 C1 C5 126.2(2) . 4_565
N1 C1 C2 109.32(19) . .
C5 C1 C2 124.4(2) 4_565 .
C3 C2 C1 107.31(19) . .
C3 C2 H2 126.3 . .
C1 C2 H2 126.3 . .
C2 C3 C4 107.3(2) . .
C2 C3 H3 126.4 . .
C4 C3 H3 126.4 . .
N1 C4 C5 126.2(2) . .
N1 C4 C3 109.42(19) . .
C5 C4 C3 124.3(2) . .
C4 C5 C1 124.1(2) . 3_655
C4 C5 C6 117.9(2) . .
C1 C5 C6 117.9(2) 3_655 .
C11 C6 C7 118.3(3) . .
C11 C6 C5 122.0(6) . .
C7 C6 C5 119.7(6) . .
C8 C7 C6 119.8(7) . .
C8 C7 H7 120.1 . .
C6 C7 H7 120.1 . .
C7 C8 C9 120.2(7) . .
C7 C8 H8 119.9 . .
C9 C8 H8 119.9 . .
C10 C9 C8 119.4(3) . .
C10 C9 H9 120.3 . .
C8 C9 H9 120.3 . .
C9 C10 C11 120.3(7) . .
C9 C10 H10 119.8 . .
C11 C10 H10 119.8 . .
C6 C11 C10 122.0(7) . .
C6 C11 H11 119.0 . .
C10 C11 H11 119.0 . .
C4 N1 C1 106.65(17) . .
C4 N1 Ti' 125.0(2) . .
C1 N1 Ti' 125.08(19) . .
C4 N1 Ti 125.21(19) . .
C1 N1 Ti 125.11(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti O1 1.575(15) .
Ti N1 2.108(3) 4_565
Ti N1 2.108(3) 2_665
Ti N1 2.108(3) 3_655
Ti N1 2.108(3) .
Ti' O1' 1.629(18) .
Ti' N1 2.104(2) 2_665
Ti' N1 2.104(2) 3_655
Ti' N1 2.104(2) 4_565
Ti' N1 2.104(2) .
C1 N1 1.373(3) .
C1 C5 1.399(3) 4_565
C1 C2 1.436(3) .
C2 C3 1.349(4) .
C2 H2 0.9300 .
C3 C4 1.435(3) .
C3 H3 0.9300 .
C4 N1 1.373(3) .
C4 C5 1.397(3) .
C5 C6 1.489(3) .
C6 C11 1.336(10) .
C6 C7 1.401(9) .
C7 C8 1.373(9) .
C7 H7 0.9300 .
C8 C9 1.397(14) .
C8 H8 0.9300 .
C9 C10 1.325(13) .
C9 H9 0.9300 .
C10 C11 1.395(9) .
C10 H10 0.9300 .
C11 H11 0.9300 .
