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

data_7710814
_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 N4 Na2'
_chemical_formula_sum            'C58 H80 Al2 N4 Na2'
_chemical_formula_weight         933.20
_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                 98.5389(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.98403(11)
_cell_length_b                   16.98245(14)
_cell_length_c                   13.13426(12)
_cell_measurement_reflns_used    14989
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      72.6080
_cell_measurement_theta_min      3.3950
_cell_volume                     2864.01(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_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   -114.00 -16.00   1.00    1.00    --  -41.69 -57.00 -30.00   98
  2  \w   -116.00 -18.00   1.00    1.00    --  -41.69 -38.00-150.00   98
  3  \w   -106.00 -22.00   1.00    1.00    --  -41.69 -38.00 120.00   84
  4  \w    -21.00  49.00   1.00    1.00    --   41.69 -77.00-150.00   70
  5  \w    119.00 177.00   1.00    3.00    --  104.37  61.00  60.00   58
  6  \w     75.00 102.00   1.00    3.00    --  104.37  61.00-180.00   27
  7  \w    112.00 137.00   1.00    3.00    --  104.37 -77.00 -30.00   25
  8  \w     79.00 106.00   1.00    3.00    --  104.37  45.00 150.00   27
  9  \w     75.00 101.00   1.00    3.00    --  104.37  61.00  60.00   26
 10  \w     75.00 101.00   1.00    3.00    --  104.37  61.00 150.00   26
 11  \w    117.00 177.00   1.00    3.00    --  104.37  61.00 150.00   60
 12  \w     32.00  84.00   1.00    3.00    --  104.37 -45.00-180.00   52
 13  \w     75.00 176.00   1.00    3.00    --  104.37  61.00-150.00  101
 14  \w     75.00 102.00   1.00    3.00    --  104.37  61.00 120.00   27
 15  \w     30.00  57.00   1.00    3.00    --  104.37 -77.00 -60.00   27
 16  \w    102.00 164.00   1.00    3.00    --  104.37 125.00 -60.00   62
 17  \w    111.00 137.00   1.00    3.00    --  104.37 -77.00 -60.00   26
 18  \w     79.00 107.00   1.00    3.00    --  104.37  45.00-180.00   28
 19  \w    103.00 147.00   1.00    3.00    --  104.37  77.00 -60.00   44
 20  \w     79.00 169.00   1.00    3.00    --  104.37  45.00 120.00   90
 21  \w    117.00 178.00   1.00    3.00    --  104.37  77.00 -90.00   61
 22  \w     29.00  98.00   1.00    3.00    --  104.37 -77.00 -30.00   69
;
_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      -0.0525626000
_diffrn_orient_matrix_UB_12      0.0542599000
_diffrn_orient_matrix_UB_13      0.0709958000
_diffrn_orient_matrix_UB_21      -0.1068021000
_diffrn_orient_matrix_UB_22      -0.0166320000
_diffrn_orient_matrix_UB_23      -0.0647041000
_diffrn_orient_matrix_UB_31      -0.0152838000
_diffrn_orient_matrix_UB_32      -0.0707183000
_diffrn_orient_matrix_UB_33      0.0696164000
_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  0.0168
_diffrn_reflns_av_unetI/netI     0.0127
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21077
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.610
_diffrn_reflns_theta_min         4.285
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.885
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.182
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
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    1.082
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.478
_exptl_crystal_size_mid          0.402
_exptl_crystal_size_min          0.361
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.033
_refine_ls_extinction_coef       0.00141(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         5602
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0433P)^2^+1.0021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0885
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5353
_reflns_number_total             5602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02111k2.cif
_cod_data_source_block           hasj220502a
_cod_database_code               7710814
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C29H40AlN2Na
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C27-C19 \\sim C27A-C19
 with sigma of 0.01
 C29-C27 \\sim C29A-C27A \\sim C28-C27 \\sim C28A-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(H1BC)=Sof(H1BD)=Sof(H1BE)=Sof(H5BD)=Sof(H5BE)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=FVAR(1)
 Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29A)=
 Sof(H29D)=Sof(H29E)=Sof(H29F)=1-FVAR(2)
 Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=Sof(H29A)=
 Sof(H29B)=Sof(H29C)=FVAR(2)
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(H1AA,H1AB), C5(H5BD,H5BE)
5.d Idealised Me refined as rotating group:
 C1(H1BC,H1BD,H1BE), C5(H5AA,H5AB,H5AC), 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              39278
_olex2_date_sample_data_collection 2022-05-02
_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 1.216
_oxdiff_exptl_absorpt_empirical_full_min 0.805