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_7037006
_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_absolute_configuration ad
_chemical_formula_moiety         'C20 H16 Al Cl2 N4, 2(Al0.5 Cl2)'
_chemical_formula_sum            'C20 H16 Al2 Cl6 N4'
_chemical_formula_weight         579.03
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-09-15
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.09.11 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
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   7.08090(10)
_cell_length_b                   38.7664(4)
_cell_length_c                   39.2286(4)
_cell_measurement_reflns_used    34463
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      67.0310
_cell_measurement_theta_min      4.4780
_cell_volume                     10768.3(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31d (release 11-02-2014 CrysAlis171 .NET)
(compiled Feb 11 2014,18:09:27)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31d (release 11-02-2014 CrysAlis171 .NET)
(compiled Feb 11 2014,18:09:27)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31d (release 11-02-2014 CrysAlis171 .NET)
(compiled Feb 11 2014,18:09:27)
;
_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    'SIR97 (Burla et al., 2007)'
_diffrn_ambient_temperature      123.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0825
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            53286
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.093
_diffrn_reflns_theta_max         67.093
_diffrn_reflns_theta_min         4.508
_exptl_absorpt_coefficient_mu    6.594
_exptl_absorpt_correction_T_max  0.486
_exptl_absorpt_correction_T_min  0.168
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31d (release 11-02-2014 CrysAlis171 .NET)
(compiled Feb 11 2014,18:09:27)
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    1.429
_exptl_crystal_description       prism
_exptl_crystal_F_000             4672
_exptl_crystal_size_max          0.4384
_exptl_crystal_size_mid          0.319
_exptl_crystal_size_min          0.1563
_refine_diff_density_max         1.228
_refine_diff_density_min         -1.048
_refine_diff_density_rms         0.127
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.00(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         4817
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.262
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0675
_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/[\s^2^(Fo^2^)+(0.0726P)^2^+270.8097P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1815
_refine_ls_wR_factor_ref         0.1817
_reflns_Friedel_coverage         0.968
_reflns_friedel_fraction_full    0.997
_reflns_friedel_fraction_max     0.997
_reflns_number_gt                4802
_reflns_number_total             4817
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03192c2.cif
_cod_data_source_block           ayt35_AlCl3bipy
_cod_depositor_comments
'Adding full bibliography for 7037006--7037016.cif.'
_cod_database_code               7037006
_shelx_estimated_absorpt_t_max   0.425
_shelx_estimated_absorpt_t_min   0.160
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.60(4) 0.40(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 Cl8A-Al3 \\sim Cl8-Al3 \\sim Cl7A-Al3 \\sim Cl7-Al3 \\sim Cl6-Al3 \\sim
Cl9-Al3 \\sim Cl6A-Al3 \\sim Al3-
 Cl9A
 with sigma of 0.02
 Cl6-Cl7 \\sim Cl6-Cl8 \\sim Cl6-Cl9 \\sim Cl7-Cl8 \\sim Cl7-Cl9 \\sim Cl8-Cl9
 with sigma of 0.02
 Cl6A-Cl7A \\sim Cl6A-Cl8A \\sim Cl6A-Cl9A \\sim Cl7A-Cl8A \\sim Cl7A-Cl9A
\\sim Cl8A-Cl9A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Cl7 \\sim Cl9A \\sim Cl9 \\sim Cl6 \\sim Cl6A \\sim Cl7A \\sim Cl8A \\sim Cl8:
within 2.5A with sigma of 0.01 and sigma for terminal atoms of 0.01
5. Others
 Fixed Sof: Al2(0.5) Cl3(0.5) Cl7A(0.25) Cl8(0.25) Cl9(0.25) Cl8A(0.25)
 Cl7(0.25) Cl6(0.25) Cl6A(0.25) Cl9A(0.25)
6.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C14(H14), C15(H15), C21(H21), C22(H22), C24(H24),
 C25(H25), C31(H31), C32(H32), C34(H34), C35(H35), C41(H41), C42(H42), C44(H44),
  C45(H45)
;
_shelx_res_checksum              20335
_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 AlCl3bipy
_olex2_submission_special_instructions 'No special instructions were received'