Alkali Metal Influences in Aluminyl Complexes
Grams, Samuel; Mai, Jonathan; Langer, Jens; Harder, Sjoerd; Dalton Transactions  (2022) –; doi:10.1039/D2DT02111K

data_7710811
_publ_section_title
;
 Alkali Metal Influences in Aluminyl Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02111K
_journal_year                    2022
_chemical_formula_moiety         'C58 H80 Al2 Li2 N4'
_chemical_formula_sum            'C58 H80 Al2 Li2 N4'
_chemical_formula_weight         901.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-21
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-06-27 deposited with the CCDC.	2022-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.304(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.6973(3)
_cell_length_b                   17.1843(6)
_cell_length_c                   12.9109(4)
_cell_measurement_reflns_used    4280
_cell_measurement_temperature    100.0(6)
_cell_measurement_theta_max      72.1350
_cell_measurement_theta_min      4.2930
_cell_volume                     2771.65(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.967
_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    -67.00  39.00   1.00    6.50    --  -40.36   0.00 -60.00  106
  2  \w     33.00  79.00   1.00    6.50    --   40.36-125.00  60.00   46
  3  \w     10.00  63.00   1.00    6.50    --   40.36 -99.00-120.00   53
  4  \w     54.00 109.00   1.00   26.00    --  104.57-111.00 -30.00   55
  5  \w     65.00 108.00   1.00   26.00    --  104.57-111.00 120.00   43
  6  \w     32.00 130.00   1.00   26.00    --  104.57 -45.00 150.00   98
  7  \w    108.00 166.00   1.00   26.00    --  104.57  77.00 -60.00   58
  8  \w    104.00 161.00   1.00   26.00    --  104.57 111.00-150.00   57
  9  \w    104.00 150.00   1.00   26.00    --  104.57  77.00 -90.00   46
 10  \w     29.00 106.00   1.00   26.00    --  104.57 -94.00 150.00   77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0039933000
_diffrn_orient_matrix_UB_12      -0.0892838000
_diffrn_orient_matrix_UB_13      0.0082840000
_diffrn_orient_matrix_UB_21      0.0792660000
_diffrn_orient_matrix_UB_22      0.0034709000
_diffrn_orient_matrix_UB_23      0.1052910000
_diffrn_orient_matrix_UB_31      -0.0944388000
_diffrn_orient_matrix_UB_32      0.0064041000
_diffrn_orient_matrix_UB_33      0.0597099000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9860
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.265
_diffrn_reflns_theta_min         4.328
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.751
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.080
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.087
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         5296
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0462P)^2^+0.5680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1139
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4266
_reflns_number_total             5296
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02111k2.cif
_cod_data_source_block           hasj211026d
_cod_original_cell_volume        2771.66(14)
_cod_database_code               7710811
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C58H80Al2Li2N4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H5a,H5b,H5c} of C5, All C(H,H) groups
 At 1.5 times of:
  {H28d,H28e,H28f} of C28A, {H29d,H29e,H29f} of C29A, {H29a,H29b,H29c} of C29,
   {H13a,H13b,H13c} of C13, {H14a,H14b,H14c} of C14, {H16a,H16b,H16c} of C16,
  {H25a,H25b,H25c} of C25, {H26a,H26b,H26c} of C26, {H28a,H28b,H28c} of C28,
  {H17a,H17b,H17c} of C17
2. Restrained distances
 C27-C23 \\sim C27A-C23
 with sigma of 0.02
 C28-C27 \\sim C28A-C27A \\sim C29-C27 \\sim C29A-C27A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C27 \\sim C28 \\sim C29 \\sim C27A \\sim C28A \\sim C29A: within 4A with sigma
of 0.02 and sigma for terminal atoms of 0.04 within 4A
4. Others
 Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28d)=Sof(H28e)=Sof(H28f)=Sof(C29A)=
 Sof(H29d)=Sof(H29e)=Sof(H29f)=1-FVAR(1)
 Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28a)=Sof(H28b)=Sof(H28c)=Sof(C29)=Sof(H29a)=
 Sof(H29b)=Sof(H29c)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C27A(H27A)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22)
5.c X=CH2 refined with riding coordinates:
 C1(H1a,H1b)
5.d Idealised Me refined as rotating group:
 C5(H5a,H5b,H5c), C13(H13a,H13b,H13c), C14(H14a,H14b,H14c), C16(H16a,H16b,
 H16c), C17(H17a,H17b,H17c), C25(H25a,H25b,H25c), C26(H26a,H26b,H26c), C28(H28a,
 H28b,H28c), C29(H29a,H29b,H29c), C28A(H28d,H28e,H28f), C29A(H29d,H29e,H29f)
;
_shelx_res_checksum              9499
_olex2_date_sample_data_collection 2021-10-26
_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 1.979
_oxdiff_exptl_absorpt_empirical_full_min 0.701