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

data_7710816
_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         'C80 H118 Al2 Cs2 N4 O4, 2(C4 H8 O)'
_chemical_formula_sum            'C88 H134 Al2 Cs2 N4 O6'
_chemical_formula_weight         1663.76
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_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                90.9024(16)
_cell_angle_beta                 94.7632(13)
_cell_angle_gamma                113.7230(15)
_cell_formula_units_Z            2
_cell_length_a                   15.07005(19)
_cell_length_b                   15.6249(3)
_cell_length_c                   20.9706(4)
_cell_measurement_reflns_used    31336
_cell_measurement_temperature    190.0(2)
_cell_measurement_theta_max      28.6710
_cell_measurement_theta_min      2.4360
_cell_volume                     4498.50(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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      190.0(2)
_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 0.882
_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    -15.00  30.00   1.00   12.50    --  -14.29 -99.00   0.00   45
  2  \w   -107.00 -61.00   1.00   12.50    --  -14.29-178.00  60.00   46
  3  \w    -65.00 -16.00   1.00   12.50    --  -14.29 111.00 -97.00   49
  4  \w    -77.00 107.00   1.00   12.50    --   15.15   0.00-180.00  184
  5  \w   -107.00 -61.00   1.00   12.50    --  -14.29-178.00   0.00   46
  6  \w    -15.00  30.00   1.00   12.50    --  -14.29 -99.00 120.00   45
  7  \w    -50.00  21.00   1.00   12.50    --  -14.29  77.00  30.00   71
  8  \w    -42.00  22.00   1.00   12.50    --  -14.29 -77.00 -60.00   64
  9  \w    -50.00  10.00   1.00   12.50    --  -14.29  77.00-180.00   60
 10  \w    -43.00 100.00   1.00   12.50    --   15.15  19.00 -30.00  143
;
_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      0.0109117000
_diffrn_orient_matrix_UB_12      0.0277555000
_diffrn_orient_matrix_UB_13      -0.0270644000
_diffrn_orient_matrix_UB_21      -0.0065381000
_diffrn_orient_matrix_UB_22      -0.0400723000
_diffrn_orient_matrix_UB_23      -0.0194107000
_diffrn_orient_matrix_UB_31      -0.0500671000
_diffrn_orient_matrix_UB_32      -0.0094720000
_diffrn_orient_matrix_UB_33      -0.0067878000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            80107
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.459
_diffrn_reflns_theta_min         1.771
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.880
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.556
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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    1.228
_exptl_crystal_description       block
_exptl_crystal_F_000             1748
_exptl_crystal_size_max          0.411
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.192
_refine_diff_density_max         1.076
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1143
_refine_ls_number_reflns         22043
_refine_ls_number_restraints     1077
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+4.3015P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1033
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17139
_reflns_number_total             22043
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02111k2.cif
_cod_data_source_block           hasj210113b
_cod_original_cell_volume        4498.49(15)
_cod_database_code               7710816
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C88H136Al2Cs2N4O6
_shelx_estimated_absorpt_t_max   0.849
_shelx_estimated_absorpt_t_min   0.714
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-C72A \\sim O2-C72 \\sim O2-C69A \\sim O2-C69 \\sim O3-C73A \\sim O3-C73
\\sim O3-C76A \\sim O3-C76 ~
 O6A-C88A \\sim O6A-C85A \\sim O6-C85 \\sim O6-C88 \\sim O5-C84 \\sim O5-C81
\\sim O5A-C84A \\sim O5A-C81A
 with sigma of 0.01
 C71-C70 \\sim C71A-C70A \\sim C75A-C74A \\sim C74-C75 \\sim C87A-C86A \\sim
C86-C87 \\sim C82-C83 ~
 C82A-C81A
 with sigma of 0.02
 C85-C87 \\sim C88-C86 \\sim C85A-C87A \\sim C88A-C86A \\sim C81-C83 \\sim
C84-C82 \\sim C84A-C82A ~
 C81A-C83A
 with sigma of 0.02
 C75-C76 \\sim C76A-C75A \\sim C74-C73 \\sim C74A-C73A \\sim C82-C81 \\sim
C84-C83 \\sim C82A-C81A ~
 C83A-C84A \\sim C70A-C69A \\sim C70-C69 \\sim C71-C72 \\sim C72A-C71A \\sim
C88A-C87A \\sim C86A-C85A
 \\sim C87-C88 \\sim C85-C86
 with sigma of 0.01
 C62A-C58 \\sim C62-C58
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O2 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C69A \\sim C70A \\sim C71A
\\sim C72A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
O3 \\sim C73 \\sim C74 \\sim C75 \\sim C76 \\sim C73A \\sim C74A \\sim C75A
\\sim C76A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
O6 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim O6A \\sim C85A \\sim C86A
\\sim C87A \\sim C88A: within 3A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 3A
O5 \\sim C81 \\sim C82 \\sim C83 \\sim C84 \\sim O5A \\sim C81A \\sim C82A
\\sim C83A \\sim C84A: within 3A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 3A
4. Others
 Sof(C69A)=Sof(H69C)=Sof(H69D)=Sof(C70A)=Sof(H70C)=Sof(H70D)=Sof(C71A)=
 Sof(H71C)=Sof(H71D)=Sof(C72A)=Sof(H72C)=Sof(H72D)=1-FVAR(1)
 Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(C71)=Sof(H71A)=
 Sof(H71B)=Sof(C72)=Sof(H72A)=Sof(H72B)=FVAR(1)
 Sof(C73A)=Sof(H73C)=Sof(H73D)=Sof(C74A)=Sof(H74C)=Sof(H74D)=Sof(C75A)=
 Sof(H75C)=Sof(H75D)=Sof(C76A)=Sof(H76C)=Sof(H76D)=1-FVAR(2)
 Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(C75)=Sof(H75A)=
 Sof(H75B)=Sof(C76)=Sof(H76A)=Sof(H76B)=FVAR(2)
 Sof(O6A)=Sof(C85A)=Sof(H85C)=Sof(H85D)=Sof(C86A)=Sof(H86C)=Sof(H86D)=
 Sof(C87A)=Sof(H87C)=Sof(H87D)=Sof(C88A)=Sof(H88C)=Sof(H88D)=1-FVAR(3)
 Sof(O6)=Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(C86)=Sof(H86A)=Sof(H86B)=Sof(C87)=
 Sof(H87A)=Sof(H87B)=Sof(C88)=Sof(H88A)=Sof(H88B)=FVAR(3)
 Sof(O5A)=Sof(C81A)=Sof(H81C)=Sof(H81D)=Sof(C82A)=Sof(H82C)=Sof(H82D)=
 Sof(C83A)=Sof(H83C)=Sof(H83D)=Sof(C84A)=Sof(H84C)=Sof(H84D)=1-FVAR(4)
 Sof(O5)=Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(C83)=
 Sof(H83A)=Sof(H83B)=Sof(C84)=Sof(H84A)=Sof(H84B)=FVAR(4)
 Sof(C62A)=Sof(H62A)=Sof(C63A)=Sof(H63D)=Sof(H63E)=Sof(H63F)=Sof(C64A)=
 Sof(H64D)=Sof(H64E)=Sof(H64F)=1-FVAR(5)
 Sof(C62)=Sof(H62)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=Sof(C64)=Sof(H64A)=
 Sof(H64B)=Sof(H64C)=FVAR(5)
 Sof(H36D)=Sof(H36E)=Sof(H40C)=Sof(H40D)=Sof(H40E)=1-FVAR(6)
 Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(H40A)=Sof(H40B)=FVAR(6)
5.a Ternary CH refined with riding coordinates:
 C18(H18), C21(H21), C30(H30), C33(H33), C47(H47), C50(H50), C59(H59),
 C62(H62), C62A(H62A)
5.b Secondary CH2 refined with riding coordinates:
 C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B), C77(H77A,
 H77B), C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B), C69(H69A,H69B),
 C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B),
  C75(H75A,H75B), C76(H76A,H76B), C69A(H69C,H69D), C70A(H70C,H70D), C71A(H71C,
 H71D), C72A(H72C,H72D), C73A(H73C,H73D), C74A(H74C,H74D), C75A(H75C,H75D),
 C76A(H76C,H76D), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,
 H84B), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B),
 C81A(H81C,H81D), C82A(H82C,H82D), C83A(H83C,H83D), C84A(H84C,H84D), C85A(H85C,
 H85D), C86A(H86C,H86D), C87A(H87C,H87D), C88A(H88C,H88D)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C9(H9), C14(H14), C15(H15), C16(H16),
 C26(H26), C27(H27), C28(H28), C38(H38), C43(H43), C44(H44), C45(H45), C55(H55),
  C56(H56), C57(H57)
5.d X=CH2 refined with riding coordinates:
 C11(H11A,H11B), C36(H36D,H36E), C40(H40A,H40B)
5.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,
 H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C40(H40C,H40D,H40E),
 C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C64(H64A,
 H64B,H64C), C63A(H63D,H63E,H63F), C64A(H64D,H64E,H64F)
;
_shelx_res_checksum              86619
_olex2_date_sample_data_collection 2021-01-13
_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 1.321
_oxdiff_exptl_absorpt_empirical_full_min 0.897