Versatile structures of group 13 metal halide complexes with 4,4'-bipy: from 1D coordination polymers to 2D and 3D metal-organic frameworks.
Sevastianova, Tatiana N.; Bodensteiner, Michael; Maulieva, Albina F.; Davydova, Elena I.; Virovets, Alexander V.; Peresypkina, Eugenia V.; Balázs, Gábor; Graßl, Christian; Seidl, Michael; Scheer, Manfred; Frenking, Gernot; Berezovskaya, Ekaterina A.; Kazakov, Igor V.; Khoroshilova, Olesya V.; Timoshkin, Alexey Y.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 20648–20658; doi:10.1039/c5dt03192c

data_7037007
_publ_section_title
;
 Versatile structures of group 13 metal halide complexes with 4,4'-bipy:
 from 1D coordination polymers to 2D and 3D metal-organic frameworks.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              20648
_journal_page_last               20658
_journal_paper_doi               10.1039/c5dt03192c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C20 H16 Al Br2 N4, Al Br4'
_chemical_formula_sum            'C20 H16 Al2 Br6 N4'
_chemical_formula_weight         845.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-09-16
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.09.15 svn.r3215 for OlexSys, GUI svn.r5093)
;
_audit_update_record
;
2015-09-23 deposited with the CCDC.
2015-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.1528(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.20393(12)
_cell_length_b                   22.3430(2)
_cell_length_c                   18.06090(16)
_cell_measurement_reflns_used    22685
_cell_measurement_temperature    123.00(14)
_cell_measurement_theta_max      66.6680
_cell_measurement_theta_min      3.8640
_cell_volume                     5328.22(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.37b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.37b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.37b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5431
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  1  \w     -1.00  88.00   1.00    2.00    --   41.44-125.00   0.00   89
  2  \w     13.00  41.00   1.00    2.00    --   41.44-125.00 -30.00   28
  3  \w     15.00 112.00   1.00    2.00    --   41.44  38.00-120.00   97
  4  \w    -28.00  67.00   1.00    2.00    --   41.44 -38.00  60.00   95
  5  \w   -121.00 -96.00   1.00    5.00    --  -83.00 125.00-180.00   25
  6  \w     83.00 109.00   1.00    5.00    --   93.50 -93.00  57.00   26
  7  \w     22.00  48.00   1.00    5.00    --   93.50 -93.00  57.00   26
  8  \w     86.00 130.00   1.00    5.00    --   93.50 -92.00 -37.00   44
  9  \w     89.00 125.00   1.00    5.00    --   93.50 -66.00 113.00   36
 10  \w     76.00 102.00   1.00    5.00    --   93.50 -91.00  18.00   26
 11  \w     20.00  48.00   1.00    5.00    --   93.50 -60.00 -97.00   28
 12  \w     63.00  89.00   1.00    5.00    --   93.50 -60.00 -97.00   26
 13  \w     34.00  59.00   1.00    5.00    --   93.50 -57.00 -26.00   25
 14  \w     60.00  96.00   1.00    5.00    --   93.50 -57.00 -26.00   36
 15  \w     44.00 131.00   1.00    5.00    --   93.50 -92.00-156.00   87
 16  \w     24.00  49.00   1.00    5.00    --   93.50 -77.00  30.00   25
 17  \w     73.00 162.00   1.00    5.00    --   93.50  77.00  90.00   89
 18  \w     29.00  55.00   1.00    5.00    --   93.50 -91.00  18.00   26
 19  \w    109.00 135.00   1.00    5.00    --   93.50 125.00  90.00   26
 20  \w     32.00  58.00   1.00    5.00    --   93.50 -45.00  30.00   26
 21  \w    138.00 164.00   1.00    5.00    --   93.50 125.00 -90.00   26
 22  \w     19.00  46.00   1.00    5.00    --   93.50 -45.00-180.00   27
 23  \w     43.00 103.00   1.00    5.00    --   93.50  15.00 150.00   60
 24  \w     88.00 113.00   1.00    5.00    --   93.50 -77.00 -90.00   25
 25  \w     26.00  52.00   1.00    5.00    --   93.50 -15.00-150.00   26
 26  \w     88.00 154.00   1.00    5.00    --   93.50 -15.00-150.00   66
 27  \w     19.00  76.00   1.00    5.00    --   93.50 -45.00 120.00   57
 28  \w     16.00  78.00   1.00    5.00    --   93.50 -77.00-120.00   62
 29  \w    101.00 126.00   1.00    5.00    --   93.50 -77.00-120.00   25
 30  \w     69.00 116.00   1.00    5.00    --   93.50 -90.00  94.00   47
 31  \w     69.00  98.00   1.00    5.00    --   93.50  77.00-180.00   29
 32  \w    115.00 159.00   1.00    5.00    --   93.50  77.00 -60.00   44
 33  \w     75.00 123.00   1.00    5.00    --   93.50 -64.00   7.00   48
 34  \w     64.00  90.00   1.00    5.00    --   93.50  77.00 -60.00   26
 35  \w    143.00 169.00   1.00    5.00    --   93.50  77.00-180.00   26
 36  \w    124.00 159.00   1.00    5.00    --   93.50 125.00-120.00   35
 37  \w     51.00  76.00   1.00    5.00    --   93.50 -45.00 -90.00   25
 38  \w     69.00  94.00   1.00    5.00    --   93.50 -77.00  30.00   25
 39  \w     21.00  46.00   1.00    5.00    --   93.50 -64.00   7.00   25
 40  \w     34.00  60.00   1.00    5.00    --   93.50  15.00 -60.00   26
 41  \w    102.00 127.00   1.00    5.00    --   93.50  15.00 -60.00   25
 42  \w    146.00 171.00   1.00    5.00    --   93.50  15.00 -60.00   25
 43  \w     75.00 100.00   1.00    5.00    --   93.50 -87.00-153.00   25
 44  \w    135.00 176.00   1.00    5.00    --   93.50  15.00-150.00   41
 45  \w     66.00 109.00   1.00    5.00    --   93.50 -15.00   0.00   43
 46  \w     91.00 116.00   1.00    5.00    --   93.50 125.00   0.00   25
 47  \w    107.00 154.00   1.00    5.00    --   93.50 125.00  60.00   47
 48  \w     11.00  37.00   1.00    5.00    --   93.50 -92.00-156.00   26
 49  \w     77.00 102.00   1.00    5.00    --   93.50 -91.00 -93.00   25
 50  \w     61.00  87.00   1.00    5.00    --   93.50 -77.00 120.00   26
 51  \w     18.00  47.00   1.00    5.00    --   93.50 -91.00 -93.00   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0517709000
_diffrn_orient_matrix_UB_12      0.0612352000
_diffrn_orient_matrix_UB_13      -0.0096996000
_diffrn_orient_matrix_UB_21      0.0828944000
_diffrn_orient_matrix_UB_22      0.0293814000
_diffrn_orient_matrix_UB_23      0.0478780000
_diffrn_orient_matrix_UB_31      0.0635249000
_diffrn_orient_matrix_UB_32      0.0116235000
_diffrn_orient_matrix_UB_33      -0.0698622000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32961
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.662
_diffrn_reflns_theta_max         66.662
_diffrn_reflns_theta_min         3.146
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.672
_exptl_absorpt_correction_T_max  0.428
_exptl_absorpt_correction_T_min  0.036
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.37b (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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.109
_exptl_crystal_description       block
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.631
_exptl_crystal_size_mid          0.381
_exptl_crystal_size_min          0.097
_refine_diff_density_max         0.695
_refine_diff_density_min         -1.265
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         4706
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0260
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+10.1722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0653
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4631
_reflns_number_total             4706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03192c2.cif
_cod_data_source_block           AlBr3bipy
_cod_depositor_comments
'Adding full bibliography for 7037006--7037016.cif.'
_cod_original_cell_volume        5328.24(9)
_cod_database_code               7037007
_chemical_oxdiff_formula         'C11 H10 N O'
_reflns_odcompleteness_completeness 98.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00J(H00J), C00K(H00K), C00L(H00L), C00N(H00N), C00Q(H00Q),
 C00R(H00R), C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X),
 C00Y(H00Y), C00Z(H00Z), C010(H010), C011(H011)
;
_shelx_res_checksum              29891
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Instruments, CryoJet'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder with inert oil'
_olex2_submission_original_sample_id AlBr3bipy
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 17.583
_oxdiff_exptl_absorpt_empirical_full_min 0.520