#------------------------------------------------------------------------------
#$Date: 2017-06-16 04:03:09 +0300 (Fri, 16 Jun 2017) $
#$Revision: 197866 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/02/7120281.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_7120281
loop_
_publ_author_name
'Mouchaham, Georges'
'Abeykoon, Brain'
'Giménez-Marqués, Mónica'
'Navalon, Sergio'
'Santiago-Portillo, Andrea'
'affram, maame'
'Guillou, Nathalie'
'Martineau, Charlotte'
'Garcia, Hermenegildo'
'Fateeva, Alexandra'
'Devic, Thomas'
_publ_section_title
;
 Adaptability of the metal(III,IV) 1,2,3-trioxobenzene rod Second-ary
 Building Unit for the production of chemically stable and catalyt-ically
 active Metal-Organic Frameworks
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC04215A
_journal_year                    2017
_chemical_formula_moiety         La2C44H24N4O12
_chemical_formula_sum            'C22 H12 La N2 O6'
_chemical_formula_weight         539.25
_chemical_name_common            La2(H6PorphGal)
_chemical_name_systematic        MIL-173(La)
_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_Hall           '-I 4 2'
_space_group_name_H-M_alt        'I 4/m m m'
_symmetry_space_group_name_Hall  '-I 4 2'
_symmetry_space_group_name_H-M   'I 4/m m m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-04-15 deposited with the CCDC.
2017-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.6040(6)
_cell_length_b                   20.6040(6)
_cell_length_c                   8.5110(6)
_cell_measurement_reflns_used    2829
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.203
_cell_measurement_theta_min      3.233
_cell_volume                     3613.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.2634
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measurement_device_type  'Xcalibur, Onyx'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.897
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6428
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.400
_diffrn_reflns_theta_min         2.589
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.206
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.75299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.991
_exptl_crystal_description       needle
_exptl_crystal_F_000             1052
_exptl_crystal_recrystallization_method 'solvothermal synthesis'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     55
_refine_ls_number_reflns         1299
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0371
_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)+(0.0456P)²+9.1343P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1059
_reflns_number_total             1299
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cc04215a2.cif
_cod_data_source_block           shelx
_cod_database_code               7120281
_shelx_shelxl_version_number     2016/6
_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'
'-y, x, z'
'y, -x, z'
'-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'
'-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'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'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'
'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
La1 La 0.500000 0.000000 0.250000 0.02907(16) Uani 1 8 d S T P
O1 O 0.500000 -0.06112(18) 0.500000 0.0370(10) Uani 1 4 d S T P
C1 C 0.500000 -0.1258(3) 0.500000 0.0361(13) Uani 1 4 d S T P
C4 C 0.500000 -0.2601(2) 0.500000 0.0363(14) Uani 1 4 d S T P
C2 C 0.500000 -0.1595(2) 0.6388(6) 0.0579(15) Uani 1 2 d S T P
C5 C 0.500000 -0.3329(3) 0.500000 0.0357(15) Uani 1 4 d S T P
C3 C 0.500000 -0.2280(2) 0.6374(7) 0.0607(16) Uani 1 2 d DS T P
H3 H 0.500000 -0.250884 0.731621 0.073 Uiso 1 2 calc R U P
O2 O 0.500000 -0.1234(2) 0.7713(4) 0.122(3) Uani 1 2 d DS T P
H2 H 0.500000 -0.1451(11) 0.852(2) 0.146 Uiso 0.75 2 d DS U P
N1 N 0.57066(16) -0.42934(16) 0.500000 0.0399(13) Uani 1 4 d S T P
H1 H 0.541149 -0.458853 0.500000 0.048 Uiso 0.5 4 calc R U P
C6 C 0.55932(19) -0.36410(19) 0.500000 0.0406(11) Uani 1 2 d S T P
C7 C 0.6214(2) -0.3330(2) 0.500000 0.0637(17) Uani 1 2 d S T P
H7 H 0.628626 -0.288428 0.500000 0.076 Uiso 1 2 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'
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
O1 La1 O1 137.78(10) . 27
O1 La1 O1 61.24(15) . 17_656
O1 La1 O1 137.78(10) 27 17_656
O1 La1 O1 137.78(10) . 11_544
O1 La1 O1 61.25(15) 27 11_544
O1 La1 O1 137.78(10) 17_656 11_544
O1 La1 O2 86.50(7) . 11_544
O1 La1 O2 124.69(11) 27 11_544
O1 La1 O2 86.50(7) 17_656 11_544
O1 La1 O2 63.45(11) 11_544 11_544
O1 La1 O2 63.45(11) . 18_556
O1 La1 O2 86.50(7) 27 18_556
O1 La1 O2 124.69(11) 17_656 18_556
O1 La1 O2 86.50(7) 11_544 18_556
O2 La1 O2 90.289(12) 11_544 18_556
O1 La1 O2 86.50(7) . 12_554
O1 La1 O2 63.45(11) 27 12_554
O1 La1 O2 86.50(7) 17_656 12_554
O1 La1 O2 124.69(11) 11_544 12_554
O2 La1 O2 171.86(17) 11_544 12_554
O2 La1 O2 90.289(12) 18_556 12_554
O1 La1 O2 124.69(11) . 17_656
O1 La1 O2 86.50(7) 27 17_656
O1 La1 O2 63.45(11) 17_656 17_656
O1 La1 O2 86.50(7) 11_544 17_656
O2 La1 O2 90.289(12) 11_544 17_656
O2 La1 O2 171.86(17) 18_556 17_656
O2 La1 O2 90.289(12) 12_554 17_656
C1 O1 La1 120.62(7) . 17_656
C1 O1 La1 120.62(7) . .
La1 O1 La1 118.76(15) 17_656 .
O1 C1 C2 120.5(3) . 18_556
O1 C1 C2 120.5(3) . .
C2 C1 C2 119.1(5) 18_556 .
C3 C4 C3 121.0(5) 18_556 .
C3 C4 C5 119.5(3) 18_556 .
C3 C4 C5 119.5(3) . .
O2 C2 C1 116.1(4) . .
O2 C2 C3 123.9(5) . .
C1 C2 C3 120.0(5) . .
C6 C5 C6 124.4(5) . 5_656
C6 C5 C4 117.8(2) . .
C6 C5 C4 117.8(2) 5_656 .
C4 C3 C2 120.0(5) . .
C4 C3 H3 120.0 . .
C2 C3 H3 120.0 . .
C2 O2 La1 119.4(3) . 17_656
C2 O2 H2 113.4(16) . .
La1 O2 H2 127.3(16) 17_656 .
C6 N1 C6 109.7(5) . 7_646
C6 N1 H1 125.1 . .
C6 N1 H1 125.1 7_646 .
N1 C6 C5 127.6(4) . .
N1 C6 C7 106.7(4) . .
C5 C6 C7 125.6(4) . .
C7 C7 C6 108.4(2) 7_646 .
C7 C7 H7 125.8 7_646 .
C6 C7 H7 125.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
La1 O1 2.4725(19) .
La1 O1 2.4726(19) 27
La1 O1 2.4726(19) 17_656
La1 O1 2.4726(19) 11_544
La1 O2 2.549(4) 11_544
La1 O2 2.549(4) 18_556
La1 O2 2.549(4) 12_554
La1 O2 2.549(4) 17_656
O1 C1 1.332(6) .
C1 C2 1.370(6) 18_556
C1 C2 1.370(6) .
C4 C3 1.344(6) 18_556
C4 C3 1.344(6) .
C4 C5 1.498(7) .
C2 O2 1.351(6) .
C2 C3 1.411(6) .
C5 C6 1.381(5) .
C5 C6 1.381(5) 5_656
C3 H3 0.9300 .
O2 H2 0.82(2) .
N1 C6 1.364(5) .
N1 C6 1.364(5) 7_646
N1 H1 0.8600 .
C6 C7 1.431(6) .
C7 C7 1.329(10) 7_646
C7 H7 0.9300 .
