Coordination polymers and molecular complexes of group 13 metal halides with bis-pyridylethane: comparison with rigid N-containing ligands
Gugin, Nikita Y.; Virovets, Alexander V.; Peresypkina, Eugenia; Davydova, Elena I.; Timoshkin, Alexey Y.; CrystEngComm  (2022) –; doi:10.1039/D2CE01063A

data_7245838
_publ_section_title
;
 Coordination polymers and molecular complexes of group 13 metal halides
 with bis-pyridylethane: comparison with rigid N-containing ligands
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01063A
_journal_year                    2022
_chemical_formula_moiety         'C60 H60 Br4 Ga2 N10, C12 H12 N2, 2(Ga Br4)'
_chemical_formula_sum            'C72 H72 Br12 Ga4 N12'
_chemical_formula_weight         2343.21
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-09-14 deposited with the CCDC.	2022-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.2974(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.30770(10)
_cell_length_b                   30.5567(3)
_cell_length_c                   13.49162(13)
_cell_measurement_reflns_used    11652
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.1030
_cell_measurement_theta_min      4.2950
_cell_volume                     4193.62(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18986
_diffrn_reflns_point_group_measured_fraction_full 0.747
_diffrn_reflns_point_group_measured_fraction_max 0.715
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         74.208
_diffrn_reflns_theta_min         3.621
_diffrn_source_type              'microfocus SuperNova source'
_exptl_absorpt_coefficient_mu    8.535
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.856
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.21a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.856
_exptl_crystal_description       prism
_exptl_crystal_F_000             2264
_exptl_crystal_size_max          0.111
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.042
_refine_diff_density_max         1.707
_refine_diff_density_min         -2.253
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.54(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     940
_refine_ls_number_reflns         12203
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0716P)^2^+6.5438P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1232
_reflns_Friedel_coverage         0.458
_reflns_Friedel_fraction_full    0.493
_reflns_Friedel_fraction_max     0.450
_reflns_number_gt                10666
_reflns_number_total             12203
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01063a2.cif
_cod_data_source_block           ayt91
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               7245838
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.451
_shelx_estimated_absorpt_t_max   0.716
_shelx_res_checksum              22653
_shelx_hkl_checksum              93395