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

data_7710815
_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 Cs2 N4, 1.264(C2.768 H3.164)'
_chemical_formula_sum            'C61.5 H84 Al2 Cs2 N4'
_chemical_formula_weight         1199.10
_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                96.6030(10)
_cell_angle_beta                 96.2390(10)
_cell_angle_gamma                96.2070(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1714(2)
_cell_length_b                   15.2939(2)
_cell_length_c                   17.2744(2)
_cell_measurement_reflns_used    29484
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      72.7050
_cell_measurement_theta_min      3.6450
_cell_volume                     3151.57(8)
_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      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.982
_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   -116.00 -17.00   0.50    1.50    --  -41.48 -38.00  90.00  198
  2  \w    -82.00  39.00   0.50    1.50    --  -41.48  19.00 -90.00  242
  3  \w    -87.00  -6.00   0.50    1.50    --  -41.48 125.00 -60.00  162
  4  \w      6.00  32.00   0.50    1.50    --   41.48  85.00  97.50   52
  5  \w     76.00 178.00   0.50    6.00    --  104.33  30.00 -90.00  204
  6  \w     22.00 106.00   0.50    6.00    --  104.33 -94.00  60.00  168
  7  \w     32.00 133.00   0.50    6.00    --  104.33 -61.00  60.00  202
  8  \w     28.00 133.00   0.50    6.00    --  104.33 -30.00-150.00  210
  9  \w     22.00 106.00   0.50    6.00    --  104.33 -94.00 -30.00  168
 10  \w     22.00 106.00   0.50    6.00    --  104.33 -94.00 150.00  168
 11  \w     31.00 130.00   0.50    6.00    --  104.33 -45.00-120.00  198
 12  \w     75.00 177.00   0.50    6.00    --  104.33  61.00-150.00  204
 13  \w     76.00 178.00   0.50    6.00    --  104.33  30.00-180.00  204
 14  \w     23.00 107.00   0.50    6.00    --  104.33 -98.00-108.10  168
 15  \w   -114.00 -13.00   0.50    1.50    --  -41.48 -57.00 -90.00  202
 16  \w      8.00  42.00   0.50    1.50    --   41.48  81.00 -13.35   68
 17  \w      8.00  42.00   0.50    1.50    --   41.48  82.00 -97.89   68
 18  \w      9.00  36.00   0.50    1.50    --   41.48  75.00-129.40   54
 19  \w     75.00 177.00   0.50    6.00    --  104.33  61.00 -30.00  204
 20  \w     75.00 177.00   0.50    6.00    --  104.33  61.00  90.00  204
 21  \w     78.00 177.00   0.50    6.00    --  104.33  45.00 -30.00  198
 22  \w     75.00 177.00   0.50    6.00    --  104.33  61.00 120.00  204
 23  \w     76.00 178.00   0.50    6.00    --  104.33  30.00  30.00  204
 24  \w     75.00 177.00   0.50    6.00    --  104.33  61.00-180.00  204
 25  \w     75.00 177.00   0.50    6.00    --  104.33  61.00 -90.00  204
 26  \w     75.00 143.00   0.50    6.00    --  104.33  61.00 -60.00  136
 27  \w     78.00 177.00   0.50    6.00    --  104.33  45.00  60.00  198
;
_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      0.1025257000
_diffrn_orient_matrix_UB_12      0.0412600000
_diffrn_orient_matrix_UB_13      -0.0339531000
_diffrn_orient_matrix_UB_21      0.0717445000
_diffrn_orient_matrix_UB_22      0.0001745000
_diffrn_orient_matrix_UB_23      0.0792008000
_diffrn_orient_matrix_UB_31      0.0282647000
_diffrn_orient_matrix_UB_32      -0.0934660000
_diffrn_orient_matrix_UB_33      -0.0275217000
_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  0.0294
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            48647
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.722
_diffrn_reflns_theta_min         2.931
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.564
_exptl_absorpt_correction_T_max  0.749
_exptl_absorpt_correction_T_min  0.367
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       block
_exptl_crystal_F_000             1234
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.074
_refine_diff_density_max         1.389
_refine_diff_density_min         -1.632
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     834
_refine_ls_number_reflns         12306
_refine_ls_number_restraints     893
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0222P)^2^+5.0617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0841
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11871
_reflns_number_total             12306
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02111k2.cif
_cod_data_source_block           hasj210202a
_cod_original_formula_sum        'C61.50 H84 Al2 Cs2 N4'
_cod_database_code               7710815
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C61.5H84Al2Cs2N4
_shelx_estimated_absorpt_t_max   0.538
_shelx_estimated_absorpt_t_min   0.278
_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
 C59-HR = C63-HS
 0.95 with sigma of 0.0001
 HC-C59 = HD-C59 = HE-C59 = HB-C63 = C63-H = C63-HA
 2.052 with sigma of 0.0001
 C65-HC = C65-HD = C65-HE = C65B-HB = C65B-H = C65B-HA
 0.98 with sigma of 0.0001
 C59-C60 \\sim C64-C59 \\sim C63-C64 \\sim C63-C62 \\sim C62-C61 \\sim C60-C61
 with sigma of 0.01
 C63-C59 \\sim C64-C60 \\sim C59-C61 \\sim C60-C62 \\sim C61-C63 \\sim C62-C64
 with sigma of 0.02
 C62-C59 \\sim C61-C64 \\sim C60-C63
 with sigma of 0.02
 C64-C65 \\sim C65-C60
 with sigma of 0.02
 C19-C24A \\sim C19-C24
 with sigma of 0.02
 C24-C25 \\sim C24A-C25A \\sim C24A-C26A \\sim C24-C26
 with sigma of 0.02
 C64A-C65A \\sim C65A-C60A
 with sigma of 0.02
 C60-HR \\sim HR-C64 \\sim C62-HS \\sim HS-C64
 with sigma of 0.001
 HC-HD \\sim HD-HE \\sim HE-HC \\sim HA-H \\sim H-HB
 with sigma of 0.001
3. Restrained planarity
 HB, C65B, C63, C64
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C19 \\sim C24A \\sim C25A \\sim C26A \\sim C24 \\sim C25 \\sim C26: within 4A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 4A
C65B \\sim C65 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64
\\sim C59A \\sim C60A \\sim C61A \\sim C62A \\sim C63A \\sim C64A \\sim C65A:
within 5A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 5A
5. Rigid body (RIGU) restrains
 C65B, C65, C59, C60, C61, C62, C63, C64
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19, C24A, C25A, C26A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C59A, C60A, C61A, C62A, C63A, C64A, C65A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(C59)+Sof(C60)+Sof(HF)+Sof(C61)+Sof(HG)+Sof(C62)+Sof(HH)+Sof(C63)+
 Sof(C64)+Sof(HI)+Sof(C59A)+Sof(C60A)+Sof(HJ)+Sof(C61A)+Sof(HK)+Sof(C62A)+
 Sof(HL)+Sof(C63A)+Sof(HM)+Sof(C64A)+Sof(HN)+Sof(C65A)+Sof(HO)+Sof(HP)+Sof(HQ)]+
 1*[Sof(C65)+Sof(HC)+Sof(HD)+Sof(HE)+Sof(HS)]+1*[Sof(C65B)+Sof(H)+Sof(HA)+
 Sof(HB)+Sof(HR)]=1 with esd of 0.0001
 Sof(C53)=Sof(H53)=Sof(C54)=Sof(H54D)=Sof(H54E)=Sof(H54F)=Sof(C55)=Sof(H55D)=
 Sof(H55E)=Sof(H55F)=1-FVAR(1)
 Sof(C53A)=Sof(H53A)=Sof(C54A)=Sof(H54A)=Sof(H54B)=Sof(H54C)=Sof(C55A)=
 Sof(H55A)=Sof(H55B)=Sof(H55C)=FVAR(1)
 Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C26)=Sof(H26D)=
 Sof(H26E)=Sof(H26F)=1-FVAR(2)
 Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26A)=
 Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(2)
 Sof(C59)=Sof(C60)=Sof(HF)=Sof(C61)=Sof(HG)=Sof(C62)=Sof(HH)=Sof(C63)=Sof(C64)=
 Sof(HI)=0.5*(1-FVAR(4))
 Sof(C59A)=Sof(C60A)=Sof(HJ)=Sof(C61A)=Sof(HK)=Sof(C62A)=Sof(HL)=Sof(C63A)=
 Sof(HM)=Sof(C64A)=Sof(HN)=Sof(C65A)=Sof(HO)=Sof(HP)=Sof(HQ)=0.5*FVAR(4)
 Sof(C65)=Sof(HC)=Sof(HD)=Sof(HE)=Sof(HS)=0.5*FVAR(5)
 Sof(C65B)=Sof(H)=Sof(HA)=Sof(HB)=Sof(HR)=0.5*FVAR(6)
 Sof(H30C)=Sof(H30D)=Sof(H30E)=Sof(H34D)=Sof(H34E)=1-FVAR(6)
 Sof(H30A)=Sof(H30B)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(6)
7.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C27(H27), C41(H41), C44(H44), C56(H56), C24A(H24A),
 C53A(H53A), C24(H24), C53(H53)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C32(H32),
 C37(H37), C38(H38), C39(H39), C49(H49), C50(H50), C51(H51), C60(HF), C61(HG),
 C62(HH), C64(HI), C60A(HJ), C61A(HK), C62A(HL), C63A(HM), C64A(HN)
7.c Fitted hexagon refined as free rotating group:
 C59A(C60A,C61A,C62A,C63A,C64A)
7.d X=CH2 refined with riding coordinates:
 C30(H30A,H30B), C34(H34D,H34E)
7.e Idealised Me refined as rotating group:
 C30(H30C,H30D,H30E), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C34(H34A,H34B,H34C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C57(H57A,H57B,H57C), C58(H58A,H58B,
 H58C), C25A(H25A,H25B,H25C), C26A(H26A,H26B,H26C), C54A(H54A,H54B,H54C),
 C55A(H55A,H55B,H55C), C25(H25D,H25E,H25F), C26(H26D,H26E,H26F), C54(H54D,H54E,
 H54F), C55(H55D,H55E,H55F), C65A(HO,HP,HQ)
;
_shelx_res_checksum              27200
_olex2_date_sample_data_collection 2021-02-02
_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 1.477
_oxdiff_exptl_absorpt_empirical_full_min 0.819