Group 13 element containing conformationally rigid "N-E-N" heteroatomic bridged [3.3](2,6)pyridinophanes (E = B, Al).
Bawari, Deependra; Negi, Chandrakala; Jaiswal, Kuldeep; Prashanth, Billa; Choudhury, Angshuman Roy; Singh, Sanjay; Chemical communications (Cambridge, England) 54 (2018) 8857–8860; doi:10.1039/c8cc05154b

data_7121976
_publ_section_title
;
 Group 13 element containing conformationally rigid &quot;N-E-N&quot;
 heteroatomic bridged [3.3](2,6)pyridinophanes (E = B, Al).
;
_journal_issue                   64
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8857
_journal_page_last               8860
_journal_paper_doi               10.1039/c8cc05154b
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C24 H48 Al2 N6 Si4'
_chemical_formula_sum            'C24 H48 Al2 N6 Si4'
_chemical_formula_weight         587.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-21 deposited with the CCDC.
2018-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.704(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2486(9)
_cell_length_b                   12.6136(7)
_cell_length_c                   16.1018(9)
_cell_measurement_reflns_used    7696
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      32.1980
_cell_measurement_theta_min      2.0560
_cell_volume                     3501.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)'
_computing_data_collection       'CrystalClear 2.0 (Rigaku, 2013)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0)2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -69.00 119.70   0.30    5.00    --   29.89  54.00   0.00  629
  2  \w    -69.00 119.70   0.30    5.00    --   29.89  54.00 120.00  629
  3  \w    -69.00 119.70   0.30    5.00    --   29.89  54.00 240.00  629
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'XtaLab mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0080040000
_diffrn_orient_matrix_UB_12      -0.0483612000
_diffrn_orient_matrix_UB_13      -0.0210373000
_diffrn_orient_matrix_UB_21      0.0356381000
_diffrn_orient_matrix_UB_22      -0.0211847000
_diffrn_orient_matrix_UB_23      0.0155614000
_diffrn_orient_matrix_UB_31      -0.0189012000
_diffrn_orient_matrix_UB_32      -0.0194289000
_diffrn_orient_matrix_UB_33      0.0354518000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_unetI/netI     0.0785
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            48197
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         32.777
_diffrn_reflns_theta_min         2.000
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.242
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.39.7f (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         12480
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1322
_refine_ls_R_factor_gt           0.0715
_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^)+(0.0724P)^2^+3.0383P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1627
_refine_ls_wR_factor_ref         0.1912
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7504
_reflns_number_total             12480
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05154b2.cif
_cod_data_source_block           3syn
_cod_depositor_comments
'Adding full bibliography for 7121972--7121976.cif.'
_cod_database_code               7121976
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C24 H48 N6 Al2 Si4'
_reflns_odcompleteness_completeness 96.45
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.70
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C21(H21), C22(H22), C23(H23)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4B,H4A,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,
 H18B,H18C), C19(H19A,H19B,H19C)
;
_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 1.896
_oxdiff_exptl_absorpt_empirical_full_min 0.730