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

data_7710810
_publ_section_title
;
 Alkali Metal Influences in Aluminyl Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02111K
_journal_year                    2022
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C37 H60 Al Li N2 O2'
_chemical_formula_sum            'C37 H60 Al Li N2 O2'
_chemical_formula_weight         598.79
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.73160(10)
_cell_length_b                   17.1793(2)
_cell_length_c                   20.4541(3)
_cell_measurement_reflns_used    7384
_cell_measurement_temperature    100.0(6)
_cell_measurement_theta_max      72.5570
_cell_measurement_theta_min      3.3190
_cell_volume                     3770.95(8)
_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  (Sheldrick, 2015)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.974
_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    -86.00 -11.00   1.00    5.00    --  -41.69 125.00-180.00   75
  2  \w    -64.00  31.00   1.00    5.00    --  -41.69  57.00  30.00   95
  3  \w     31.00 100.00   1.00   20.00    --  104.37-125.00 -60.00   69
  4  \w     22.00 105.00   1.00   20.00    --  104.37 -94.00  30.00   83
  5  \w    121.00 162.00   1.00   20.00    --  104.37  77.00  90.00   41
  6  \w    103.00 178.00   1.00   20.00    --  104.37  77.00-180.00   75
  7  \w     41.00 157.00   1.00   20.00    --  104.37 -15.00   0.00  116
;
_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      -0.0086059000
_diffrn_orient_matrix_UB_12      0.0882449000
_diffrn_orient_matrix_UB_13      -0.0127342000
_diffrn_orient_matrix_UB_21      0.1226308000
_diffrn_orient_matrix_UB_22      -0.0032377000
_diffrn_orient_matrix_UB_23      -0.0390377000
_diffrn_orient_matrix_UB_31      -0.0740658000
_diffrn_orient_matrix_UB_32      -0.0159188000
_diffrn_orient_matrix_UB_33      -0.0631083000
_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  0.0302
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13066
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.623
_diffrn_reflns_theta_min         3.360
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.694
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.530
_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    1.055
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.202
_exptl_crystal_size_min          0.127
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(6)
_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     520
_refine_ls_number_reflns         7208
_refine_ls_number_restraints     674
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0711P)^2^+0.5645P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1286
_reflns_Friedel_coverage         0.767
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.946
_reflns_number_gt                6400
_reflns_number_total             7208
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02111k2.cif
_cod_data_source_block           hasj210908b
_cod_database_code               7710810
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C37H60AlLiN2O2
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.793
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.51(6)
 0.49(6)
2. 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, All C(H,H,H,H,H) groups
3. Restrained distances
 C30A-C31A \\sim C31-C30 \\sim C32-C33 \\sim C33B-C32B \\sim C33A-C32A \\sim
C35-C34 \\sim C35A-C34A ~
 C37-C36 \\sim C37A-C36A
 with sigma of 0.02
 O1A-C30A \\sim O1-C30 \\sim O1-C32B \\sim O1-C32 \\sim O1A-C32A \\sim O2-C34
\\sim O2A-C34A \\sim O2-C36
 \\sim O2A-C36A
 with sigma of 0.02
 C32B-C30 \\sim C30-C32
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O1 \\sim C30 \\sim C31 \\sim O1A \\sim C30A \\sim C31A \\sim C32A \\sim C33A
\\sim C32B \\sim C33B \\sim C32 \\sim C33: within 4A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 4A
O2 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim O2A \\sim C34A \\sim C35A
\\sim C36A \\sim C37A: within 4A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 4A
5. Others
 1*[Sof(O1)+Sof(C30)+Sof(H30a)+Sof(H30b)+Sof(C31)+Sof(H31a)+Sof(H31b)+
 Sof(H31c)+Sof(O1A)+Sof(C30A)+Sof(H30c)+Sof(H30d)+Sof(C31A)+Sof(H31d)+Sof(H31e)+
 Sof(H31f)+Sof(C32A)+Sof(H32a)+Sof(H32b)+Sof(C33A)+Sof(H33a)+Sof(H33b)+
 Sof(H33c)]+1*[Sof(C32B)+Sof(H32c)+Sof(H32d)+Sof(C33B)+Sof(H33d)+Sof(H33e)+
 Sof(H33f)]+1*[Sof(C32)+Sof(H32e)+Sof(H32f)+Sof(C33)+Sof(H33g)+Sof(H33h)+
 Sof(H33i)]=1 with esd of 0.00001
 Sof(O1)=Sof(C30)=Sof(H30a)=Sof(H30b)=Sof(C31)=Sof(H31a)=Sof(H31b)=Sof(H31c)=1-
 FVAR(1)
 Sof(O1A)=Sof(C30A)=Sof(H30c)=Sof(H30d)=Sof(C31A)=Sof(H31d)=Sof(H31e)=
 Sof(H31f)=Sof(C32A)=Sof(H32a)=Sof(H32b)=Sof(C33A)=Sof(H33a)=Sof(H33b)=
 Sof(H33c)=FVAR(1)
 Sof(O2A)=Sof(C34A)=Sof(H34c)=Sof(H34d)=Sof(C35A)=Sof(H35d)=Sof(H35e)=
 Sof(H35f)=Sof(C36A)=Sof(H36c)=Sof(H36d)=Sof(C37A)=Sof(H37d)=Sof(H37e)=
 Sof(H37f)=1-FVAR(2)
 Sof(O2)=Sof(C34)=Sof(H34a)=Sof(H34b)=Sof(C35)=Sof(H35a)=Sof(H35b)=Sof(H35c)=
 Sof(C36)=Sof(H36a)=Sof(H36b)=Sof(C37)=Sof(H37a)=Sof(H37b)=Sof(H37c)=FVAR(2)
 Sof(C32B)=Sof(H32c)=Sof(H32d)=Sof(C33B)=Sof(H33d)=Sof(H33e)=Sof(H33f)=FVAR(3)
 Sof(C32)=Sof(H32e)=Sof(H32f)=Sof(C33)=Sof(H33g)=Sof(H33h)=Sof(H33i)=FVAR(4)
 Sof(H1aa)=Sof(H1ab)=Sof(H1ac)=Sof(H5bd)=Sof(H5be)=1-FVAR(5)
 Sof(H1bd)=Sof(H1be)=Sof(H5aa)=Sof(H5ac)=Sof(H5ab)=FVAR(5)
6.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27)
6.b Secondary CH2 refined with riding coordinates:
 C30(H30a,H30b), C34(H34a,H34b), C36(H36a,H36b), C30A(H30c,H30d), C32A(H32a,
 H32b), C34A(H34c,H34d), C36A(H36c,H36d), C32B(H32c,H32d), C32(H32e,H32f)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22)
6.d X=CH2 refined with riding coordinates:
 C1(H1bd,H1be), C5(H5bd,H5be)
6.e Idealised Me refined with riding coordinates:
 C31A(H31d,H31e,H31f)
6.f Idealised Me refined as rotating group:
 C1(H1aa,H1ab,H1ac), C5(H5aa,H5ac,H5ab), 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), C31(H31a,H31b,H31c),
 C35(H35a,H35b,H35c), C37(H37a,H37b,H37c), C33A(H33a,H33b,H33c), C35A(H35d,H35e,
 H35f), C37A(H37d,H37e,H37f), C33B(H33d,H33e,H33f), C33(H33g,H33h,H33i)
;
_shelx_res_checksum              7516
_olex2_date_sample_data_collection 2021-09-08
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.113
_oxdiff_exptl_absorpt_empirical_full_min 0.628