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

data_7710813
_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         'C39 H66 Al N4 Na O, 0.5(C4 H10 O)'
_chemical_formula_sum            'C41 H71 Al N4 Na O1.5'
_chemical_formula_weight         693.98
_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'
_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                 114.3945(17)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.4823(3)
_cell_length_b                   20.6133(3)
_cell_length_c                   21.7946(3)
_cell_measurement_reflns_used    45194
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      74.5700
_cell_measurement_theta_min      2.9930
_cell_volume                     8789.5(2)
_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 2018/2 (Sheldrick, 2018)'
_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 0.985
_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    -94.00 -67.00   1.00    4.00    --  -41.69 -38.00  30.00   27
  2  \w    -49.00 -22.00   1.00    4.00    --  -41.69 -57.00 -30.00   27
  3  \w    -43.00 -16.00   1.00    4.00    --  -41.69 -57.00   0.00   27
  4  \w    -75.00  -8.00   1.00    4.00    --  -41.69 125.00-120.00   67
  5  \w    -67.00 -19.00   1.00    4.00    --  -41.69 -38.00 -30.00   48
  6  \w   -114.00 -21.00   1.00    4.00    --  -41.69 -57.00 -60.00   93
  7  \w     44.00  71.00   1.00    4.00    --   41.69  57.00   0.00   27
  8  \w     33.00  96.00   1.00    4.00    --   41.69-125.00-180.00   63
  9  \w    -33.00  65.00   1.00    4.00    --   41.69 -38.00 150.00   98
 10  \w     31.00  66.00   1.00    4.00    --   41.69  38.00   0.00   35
 11  \w     26.00 107.00   1.00   16.00    --  107.95 -94.00-120.00   81
 12  \w     79.00 105.00   1.00   16.00    --  107.95  61.00  30.00   26
 13  \w    119.00 178.00   1.00   16.00    --  107.95  61.00  30.00   59
 14  \w     79.00 105.00   1.00   16.00    --  107.95  61.00   0.00   26
 15  \w     82.00 109.00   1.00   16.00    --  107.95  45.00   0.00   27
 16  \w    153.00 178.00   1.00   16.00    --  107.95  30.00   0.00   25
 17  \w    136.00 168.00   1.00   16.00    --  107.95  61.00  60.00   32
 18  \w     41.00 107.00   1.00   16.00    --  107.95 -94.00 -30.00   66
 19  \w     83.00 110.00   1.00   16.00    --  107.95  45.00 -30.00   27
 20  \w     82.00 110.00   1.00   16.00    --  107.95  45.00  30.00   28
 21  \w     83.00 108.00   1.00   16.00    --  107.95  45.00  90.00   25
 22  \w     82.00 110.00   1.00   16.00    --  107.95  45.00  60.00   28
 23  \w     80.00 107.00   1.00   16.00    --  107.95  30.00   0.00   27
 24  \w    106.00 134.00   1.00   16.00    --  107.95 111.00 150.00   28
 25  \w    141.00 168.00   1.00   16.00    --  107.95 111.00 150.00   27
 26  \w     57.00 128.00   1.00   16.00    --  107.95 -30.00   0.00   71
 27  \w     83.00 109.00   1.00   16.00    --  107.95  45.00 120.00   26
 28  \w     81.00 119.00   1.00   16.00    --  107.95  61.00 -60.00   38
 29  \w     82.00 110.00   1.00   16.00    --  107.95  30.00  30.00   28
 30  \w     80.00 107.00   1.00   16.00    --  107.95  30.00 120.00   27
 31  \w     79.00 105.00   1.00   16.00    --  107.95  61.00  90.00   26
 32  \w     84.00 111.00   1.00   16.00    --  107.95  30.00  60.00   27
 33  \w    137.00 176.00   1.00   16.00    --  107.95  61.00 -30.00   39
 34  \w    113.00 138.00   1.00   16.00    --  107.95  30.00 120.00   25
 35  \w     79.00 106.00   1.00   16.00    --  107.95  61.00 -30.00   27
 36  \w    123.00 178.00   1.00   16.00    --  107.95  61.00 -60.00   55
 37  \w     80.00 107.00   1.00   16.00    --  107.95  61.00 120.00   27
 38  \w     39.00 104.00   1.00   16.00    --  107.95-111.00-180.00   65
 39  \w     79.00 105.00   1.00   16.00    --  107.95  61.00  60.00   26
;
_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      0.0723731000
_diffrn_orient_matrix_UB_12      0.0225027000
_diffrn_orient_matrix_UB_13      0.0115315000
_diffrn_orient_matrix_UB_21      -0.0241899000
_diffrn_orient_matrix_UB_22      0.0109703000
_diffrn_orient_matrix_UB_23      -0.0762885000
_diffrn_orient_matrix_UB_31      -0.0193421000
_diffrn_orient_matrix_UB_32      0.0704431000
_diffrn_orient_matrix_UB_33      0.0082147000
_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  0.0256
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            81308
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.571
_diffrn_reflns_theta_min         3.091
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.485
_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 light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.049
_exptl_crystal_description       block
_exptl_crystal_F_000             3048
_exptl_crystal_size_max          0.401
_exptl_crystal_size_mid          0.268
_exptl_crystal_size_min          0.203
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1004
_refine_ls_number_reflns         17734
_refine_ls_number_restraints     523
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+2.8986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1089
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15751
_reflns_number_total             17734
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02111k2.cif
_cod_data_source_block           hasj220328b
_cod_original_formula_sum        'C41 H71 Al N4 Na O1.50'
_cod_database_code               7710813
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C41H71AlN4NaO1.5
_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
 C82-C81 \\sim C82A-C81A \\sim C80-C79 \\sim C80A-C79A
 with sigma of 0.02
 O3-C81 \\sim O3A-C81A \\sim O3A-C79A \\sim O3-C79
 with sigma of 0.02
 C39-C38 \\sim C39A-C38A \\sim C37-C36 \\sim C36A-C37A
 with sigma of 0.02
 O1-C36 \\sim O1A-C36A \\sim O1-C38 \\sim O1A-C38A
 with sigma of 0.02
 Na1-O1 \\sim Na1-O1A
 with sigma of 0.02
 C37A-O1A \\sim O1A-C39A \\sim C37-O1 \\sim O1-C39
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O3 \\sim C79 \\sim C80 \\sim C81 \\sim C82 \\sim O3A \\sim C79A \\sim C81A
\\sim C82A \\sim C80A: within 4A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 4A
O1 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim O1A \\sim C38A \\sim C36A
\\sim C39A \\sim C37A: within 4A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 4A
4. Others
 Sof(O3A)=Sof(C79A)=Sof(H79c)=Sof(H79d)=Sof(C81A)=Sof(H81c)=Sof(H81d)=
 Sof(C82A)=Sof(H82d)=Sof(H82e)=Sof(H82f)=Sof(C80A)=Sof(H80d)=Sof(H80e)=
 Sof(H80f)=1-FVAR(1)
 Sof(O3)=Sof(C79)=Sof(H79a)=Sof(H79b)=Sof(C80)=Sof(H80a)=Sof(H80b)=Sof(H80c)=
 Sof(C81)=Sof(H81a)=Sof(H81b)=Sof(C82)=Sof(H82a)=Sof(H82b)=Sof(H82c)=FVAR(1)
 Sof(H40c)=Sof(H40d)=Sof(H40e)=Sof(H44d)=Sof(H44e)=1-FVAR(2)
 Sof(H40a)=Sof(H40b)=Sof(H44a)=Sof(H44b)=Sof(H44c)=FVAR(2)
 Sof(O1A)=Sof(C38A)=Sof(H38c)=Sof(H38d)=Sof(C36A)=Sof(H36c)=Sof(H36d)=
 Sof(C39A)=Sof(H39d)=Sof(H39e)=Sof(H39f)=Sof(C37A)=Sof(H37d)=Sof(H37e)=
 Sof(H37f)=1-FVAR(3)
 Sof(O1)=Sof(C36)=Sof(H36a)=Sof(H36b)=Sof(C37)=Sof(H37a)=Sof(H37b)=Sof(H37c)=
 Sof(C38)=Sof(H38a)=Sof(H38b)=Sof(C39)=Sof(H39a)=Sof(H39b)=Sof(H39c)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C51(H51), C54(H54), C63(H63), C66(H66)
5.b Secondary CH2 refined with riding coordinates:
 C32(H32a,H32b), C33(H33a,H33b), C36(H36a,H36b), C38(H38a,H38b), C38A(H38c,
 H38d), C36A(H36c,H36d), C71(H71a,H71b), C72(H72a,H72b), C75(H75a,H75b),
 C77(H77a,H77b), C79(H79a,H79b), C81(H81a,H81b), C79A(H79c,H79d), C81A(H81c,
 H81d)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C42(H42),
 C47(H47), C48(H48), C49(H49), C59(H59), C60(H60), C61(H61)
5.d X=CH2 refined with riding coordinates:
 C1(H1a,H1b), C40(H40a,H40b), C44(H44d,H44e)
5.e 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), C30(H30a,H30b,H30c), C31(H31a,H31b,H31c),
 C34(H34a,H34b,H34c), C35(H35a,H35b,H35c), C37(H37a,H37b,H37c), C39(H39a,H39b,
 H39c), C39A(H39d,H39e,H39f), C37A(H37d,H37e,H37f), C40(H40c,H40d,H40e),
 C44(H44a,H44b,H44c), C52(H52a,H52b,H52c), C53(H53a,H53b,H53c), C55(H55a,H55b,
 H55c), C56(H56a,H56b,H56c), C64(H64a,H64b,H64c), C65(H65a,H65b,H65c), C67(H67a,
 H67b,H67c), C68(H68a,H68b,H68c), C69(H69a,H69b,H69c), C70(H70a,H70b,H70c),
 C73(H73a,H73b,H73c), C74(H74a,H74b,H74c), C76(H76a,H76b,H76c), C78(H78a,H78b,
 H78c), C80(H80a,H80b,H80c), C82(H82a,H82b,H82c), C82A(H82d,H82e,H82f),
 C80A(H80d,H80e,H80f)
;
_shelx_res_checksum              84835
_olex2_date_sample_data_collection 2022-03-28
_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 1.360
_oxdiff_exptl_absorpt_empirical_full_min 0.808