# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_S26
_database_code_depnum_ccdc_archive 'CCDC 1934522'
loop_
_audit_author_name
_audit_author_address
'Vladimir Chernyshev'
;Lomonosov Moscow State University
Russia
;
_audit_update_record             
;
2019-06-18 deposited with the CCDC.	2019-09-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'catena-((μ₄-2aminobenzene-1,4-dicarboxylato)-(μ₂-oxo)-aluminium)dimethylformamide solvate hydrate'


_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H5 Al N O5, C3 H7 N O, H2 O'
_chemical_formula_sum            'C11 H14 Al N2 O7'
_chemical_formula_weight         313.22

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Al Al 0.0406 0.0313 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0015 0.0009 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'I 2/m'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   6.6264(9)
_cell_length_b                   17.7350(18)
_cell_length_c                   11.2621(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.311(9)
_cell_angle_gamma                90.00
_cell_volume                     1323.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    337
_cell_measurement_theta_min      1.360
_cell_measurement_theta_max      9.998

_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             652
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

# The next three fields give the specimen dimensions in mm.  The equatorial 
# plane contains the incident and diffracted beam.
_pd_spec_size_axial              15 # perpendicular to 
# equatorial plane

_pd_spec_size_equat              1.0 # parallel to 
# scattering vector 
# in transmission

_pd_spec_size_thick              1.0 # parallel to 
# scattering vector 
# in reflection

# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                
; 
Specimen was sealed in a 1.0 mm diameter borosilicate glass capillary
;
_pd_spec_mount_mode              transmission # options are 'reflection' 
# or 'transmission'

_pd_spec_shape                   cylinder # options are 'cylinder',
# 'flat_sheet' or 'irregular'

_pd_char_particle_morphology     'no specific habit'
_pd_char_colour                  colorless # use ICDD colour descriptions

# The following three fields describe the preparation of the specimen. 
# The cooling rate is in K/min.  The pressure at which the sample was
# prepared is in kPa.  The temperature of preparation is in K.



_pd_prep_cool_rate               ?
_pd_prep_pressure                101
_pd_prep_temperature             298(2)




# 7. EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# This following item is used to identify the equipment used to record the
# powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; 
ID31 beam line, ESRF, Grenoble, France
;

_diffrn_ambient_temperature      200(2)
_diffrn_source                   'ID22 bending magnet at ESRF'
_diffrn_source_target            ?
_diffrn_source_type              'synchrotron radiation'
_diffrn_measurement_device_type  'ESRF powder diffractometer'
_diffrn_detector                 ?
_diffrn_detector_type            'scintillation counter'
_pd_meas_scan_method             cont # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         ?

# The following six items are used for angular dispersive measurements only.

_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.450851(3)
_diffrn_radiation_monochromator  'Si 111 double crystal'

# The following four items give details of the measured (not processed)
# powder pattern.  Angles are in degrees.

_pd_meas_number_of_points        9251
_pd_meas_2theta_range_min        1.500
_pd_meas_2theta_range_max        20.000
_pd_meas_2theta_range_inc        0.002

# The following fields are used to identify the programs used.

_computing_data_collection       'local program'
_computing_cell_refinement       ?
_computing_data_reduction        'MRIA (Zlokazov et al., 1992)'
_computing_structure_solution    MRIA
_computing_structure_refinement  MRIA
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL-97 and MRIA'


#==============================================================================

# 8. REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
;
Two-phases Rietveld refinement!!!
All indicators - R-factors, No. of parameters, restraints etc. - 
are given for the two-phases refinement
;

# The next three items are given as text
_pd_proc_ls_profile_function     'split-type pseudo-Voigt (Toraya, 1986)'
_pd_proc_ls_background_function  'Chebyshev polynomial up to the 5th order'
_pd_proc_ls_pref_orient_corr     none

_pd_proc_ls_prof_R_factor        0.0500
_pd_proc_ls_prof_wR_factor       0.0625
_pd_proc_ls_prof_wR_expected     0.0437

_refine_special_details          
; 
Two-phases Rietveld refinement!!!
;

_refine_ls_R_I_factor            0.1213
_refine_ls_structure_factor_coef Inet
_refine_ls_matrix_type           fullcycle
_refine_ls_weighting_scheme      sigma
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_parameters     123
_refine_ls_number_restraints     125
_refine_ls_number_constraints    17
# The following item is the same as CHI, the square root of 'CHI squared =1.946'
_refine_ls_goodness_of_fit_all   1.395

_refine_ls_restrained_S_all      ?
_refine_ls_restrained_S_obs      ?
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001


# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the 
# intensities used in the refinement.
_pd_proc_2theta_range_min        1.500
_pd_proc_2theta_range_max        20.000
_pd_proc_2theta_range_inc        0.002

_pd_proc_wavelength              0.450851(3)

_pd_block_diffractogram_id       S26_pattern # The id used for the block
#                                              # containing the powder 
#                                             # pattern profile (section 11).

# Give appropriate details in the next two text fields.
_pd_proc_info_excluded_regions   ?
_pd_proc_info_data_reduction     ?

#==============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group


Al1 Al 0.0000 0.0000 0.0000 0.065(3) Uiso 1 4 d S . .
Al2 Al 0.5000 0.0000 0.0000 0.065(3) Uiso 1 4 d S . .
O1 O 0.9196(10) 0.4228(4) 0.3956(5) 0.065(3) Uiso 1 1 d . . .
O2 O 0.5883(11) 0.4208(4) 0.3896(5) 0.065(3) Uiso 1 1 d . . .
C1 C 0.5692(15) 0.2279(6) 0.1959(8) 0.065(3) Uiso 1 1 d . . .
C2 C 0.7619(14) 0.3186(7) 0.3104(8) 0.065(3) Uiso 1 1 d . . .
C3 C 0.9171(15) 0.2017(6) 0.2483(9) 0.065(3) Uiso 1 1 d . . .
H3 H 1.0260 0.1686 0.2503 0.078 Uiso 1 1 calc . . .
C4 C 0.7572(15) 0.3905(6) 0.3684(8) 0.065(3) Uiso 1 1 d . . .
N1 N 0.382(2) 0.2110(9) 0.1421(12) 0.065(3) Uiso 0.50 1 d P . .
H1A H 0.3667 0.1699 0.1026 0.078 Uiso 0.50 1 calc P . .
H1B H 0.2821 0.2418 0.1489 0.078 Uiso 0.50 1 calc P . .
O3 O 0.2428(14) 0.0000 0.0758(8) 0.065(3) Uiso 1 2 d S . .
H31 H 0.2428 0.0000 0.1520 0.097 Uiso 1 2 d S . .
O4 O 0.717(2) 0.0719(10) 0.7201(13) 0.110(9) Uiso 0.50 1 d P . .
C5 C 0.817(3) 0.0452(11) 0.4118(16) 0.110(9) Uiso 0.50 1 d P . .
H5A H 0.7841 0.0785 0.3473 0.166 Uiso 0.50 1 d P . .
H5B H 0.7618 0.0000 0.3963 0.166 Uiso 1 2 d S . .
H5C H 0.9608 0.0417 0.4200 0.166 Uiso 0.50 1 d P . .
N2 N 0.732(3) 0.0749(10) 0.5214(16) 0.110(9) Uiso 0.50 1 d P . .
C6 C 0.756(3) 0.0391(11) 0.6231(15) 0.110(9) Uiso 0.50 1 d P . .
H6 H 0.8017 -0.0104 0.6234 0.132 Uiso 0.50 1 d P . .
C7 C 0.614(3) 0.1435(11) 0.515(2) 0.110(9) Uiso 0.50 1 d P . .
H7A H 0.6123 0.1617 0.4351 0.166 Uiso 0.50 1 d P . .
H7B H 0.6739 0.1807 0.5663 0.166 Uiso 0.50 1 d P . .
H7C H 0.4788 0.1333 0.5406 0.166 Uiso 0.50 1 d P . .
O5 O 0.092(2) 0.5939(8) 0.0113(16) 0.110(9) Uiso 0.50 1 d P . .
H5D H 0.1794 0.6288 0.0041 0.166 Uiso 0.50 1 d P . .
H5E H 0.1540 0.5544 0.0374 0.166 Uiso 0.50 1 d P . .

_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Al1 O3 1.817(9) 5 ?
Al1 O3 1.817(9) . ?
Al1 O2 1.967(6) 3_444 ?
Al1 O2 1.967(6) 7 ?
Al1 O2 1.967(6) 4_545 ?
Al1 O2 1.967(6) 8_454 ?
Al2 O1 1.880(6) 7_655 ?
Al2 O1 1.880(6) 3_444 ?
Al2 O1 1.880(6) 8_454 ?
Al2 O1 1.880(6) 4_645 ?
Al2 O3 1.910(9) 5_655 ?
Al2 O3 1.910(9) . ?
O1 C4 1.255(12) . ?
O1 Al2 1.880(6) 3 ?
O2 C4 1.266(12) . ?
O2 Al1 1.967(6) 3 ?
C1 C2 1.393(15) 7_655 ?
C1 C3 1.400(14) 7_655 ?
C1 N1 1.413(19) . ?
C2 C1 1.393(15) 7_655 ?
C2 C3 1.402(14) 7_655 ?
C2 C4 1.433(16) . ?
C3 C1 1.399(14) 7_655 ?
C3 C2 1.402(14) 7_655 ?
O4 C6 1.26(2) . ?
C5 N2 1.46(3) . ?
N2 C6 1.32(3) . ?
N2 C7 1.45(3) . ?

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
O3 Al1 O3 180.0(5) 5 . ?
O3 Al1 O2 88.2(3) 5 3_444 ?
O3 Al1 O2 91.8(3) . 3_444 ?
O3 Al1 O2 91.8(3) 5 7 ?
O3 Al1 O2 88.2(3) . 7 ?
O2 Al1 O2 180.0(5) 3_444 7 ?
O3 Al1 O2 91.8(3) 5 4_545 ?
O3 Al1 O2 88.2(3) . 4_545 ?
O2 Al1 O2 88.9(4) 3_444 4_545 ?
O2 Al1 O2 91.1(4) 7 4_545 ?
O3 Al1 O2 88.2(3) 5 8_454 ?
O3 Al1 O2 91.8(3) . 8_454 ?
O2 Al1 O2 91.1(4) 3_444 8_454 ?
O2 Al1 O2 88.9(4) 7 8_454 ?
O2 Al1 O2 180.0(5) 4_545 8_454 ?
O1 Al2 O1 180.0(4) 7_655 3_444 ?
O1 Al2 O1 86.5(4) 7_655 8_454 ?
O1 Al2 O1 93.5(4) 3_444 8_454 ?
O1 Al2 O1 93.5(4) 7_655 4_645 ?
O1 Al2 O1 86.5(4) 3_444 4_645 ?
O1 Al2 O1 180.0(5) 8_454 4_645 ?
O1 Al2 O3 91.7(3) 7_655 5_655 ?
O1 Al2 O3 88.3(3) 3_444 5_655 ?
O1 Al2 O3 88.3(3) 8_454 5_655 ?
O1 Al2 O3 91.7(3) 4_645 5_655 ?
O1 Al2 O3 88.3(3) 7_655 . ?
O1 Al2 O3 91.7(3) 3_444 . ?
O1 Al2 O3 91.7(3) 8_454 . ?
O1 Al2 O3 88.3(3) 4_645 . ?
O3 Al2 O3 180.0(5) 5_655 . ?
C4 O1 Al2 136.5(6) . 3 ?
C4 O2 Al1 133.5(6) . 3 ?
C2 C1 C3 120.1(9) 7_655 7_655 ?
C2 C1 N1 123.9(11) 7_655 . ?
C3 C1 N1 115.9(10) 7_655 . ?
C1 C2 C3 120.1(10) 7_655 7_655 ?
C1 C2 C4 124.8(9) 7_655 . ?
C3 C2 C4 115.1(9) 7_655 . ?
C1 C3 C2 119.6(10) 7_655 7_655 ?
O1 C4 O2 121.2(9) . . ?
O1 C4 C2 119.8(9) . . ?
O2 C4 C2 119.0(9) . . ?
Al1 O3 Al2 125.4(5) . . ?
C6 N2 C7 120.6(18) . . ?
C6 N2 C5 121.1(16) . . ?
C7 N2 C5 118.3(18) . . ?
O4 C6 N2 120.3(18) . . ?

_refine_diff_density_max         0.47
_refine_diff_density_min         -0.43
_refine_diff_density_rms         0.27
