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

data_7710812
_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 Rb2, 4(C7 H8)'
_chemical_formula_sum            'C86 H112 Al2 N4 Rb2'
_chemical_formula_weight         1426.69
_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   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                71.822(3)
_cell_angle_beta                 72.863(3)
_cell_angle_gamma                69.306(3)
_cell_formula_units_Z            1
_cell_length_a                   12.6926(4)
_cell_length_b                   12.8395(4)
_cell_length_c                   14.2842(5)
_cell_measurement_reflns_used    12756
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      71.1360
_cell_measurement_theta_min      3.2960
_cell_volume                     2023.95(12)
_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(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 0.983
_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    -84.00  -2.00   1.00    1.35    --  -40.36 120.00  21.00   82
  2  \w    -59.00  34.00   1.00    1.35    --  -40.36  38.00 -60.00   93
  3  \w    -84.00  -6.00   1.00    1.35    --  -40.36 125.00 -60.00   78
  4  \w   -113.00 -16.00   1.00    1.35    --  -40.36 -57.00 150.00   97
  5  \w     47.00 128.00   1.00    5.41    --  104.57 -77.00 150.00   81
  6  \w     70.00 142.00   1.00    5.41    --  104.57 178.00 120.00   72
  7  \w    131.00 177.00   1.00    5.41    --  104.57  77.00 120.00   46
  8  \w     27.00 152.00   1.00    5.41    --  104.57 -15.00  30.00  125
  9  \w     41.00 109.00   1.00    5.41    --  104.57-111.00  90.00   68
 10  \w     47.00 109.00   1.00    5.41    --  104.57-111.00 -30.00   62
 11  \w     84.00 172.00   1.00    5.41    --  104.57  45.00-150.00   88
 12  \w     38.00 112.00   1.00    5.41    --  104.57 -61.00  60.00   74
 13  \w     32.00 131.00   1.00    5.41    --  104.57 -30.00-180.00   99
 14  \w     83.00 109.00   1.00    5.41    --  104.57-111.00 150.00   26
 15  \w   -113.00 -13.00   1.00    1.35    --  -40.86 -57.00-150.00  100
 16  \w   -113.00 -13.00   1.00    1.35    --  -40.86 -57.00 -60.00  100
 17  \w   -113.00 -13.00   1.00    1.35    --  -40.86 -57.00  30.00  100
 18  \w      6.00  82.00   1.00    1.35    --   40.86 -99.00 150.00   76
 19  \w     75.00 177.00   1.00    5.41    --  104.57  61.00 -60.00  102
 20  \w     75.00 177.00   1.00    5.41    --  104.57  61.00 -90.00  102
 21  \w     75.00 177.00   1.00    5.41    --  104.57  61.00   0.00  102
 22  \w     75.00 177.00   1.00    5.41    --  104.57  61.00-120.00  102
 23  \w     52.00 178.00   1.00    5.41    --  104.57  15.00 120.00  126
 24  \w     75.00 177.00   1.00    5.41    --  104.57  61.00  90.00  102
 25  \w     75.00 177.00   1.00    5.41    --  104.57  61.00 -30.00  102
 26  \w     75.00 177.00   1.00    5.41    --  104.57  61.00 150.00  102
 27  \w   -113.00 -13.00   1.00    1.35    --  -40.86 -57.00  90.00  100
;
_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      0.0536281000
_diffrn_orient_matrix_UB_12      0.0531895000
_diffrn_orient_matrix_UB_13      -0.1083615000
_diffrn_orient_matrix_UB_21      0.0272808000
_diffrn_orient_matrix_UB_22      0.0844156000
_diffrn_orient_matrix_UB_23      0.0394399000
_diffrn_orient_matrix_UB_31      0.1181929000
_diffrn_orient_matrix_UB_32      -0.0862375000
_diffrn_orient_matrix_UB_33      0.0130146000
_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  0.0292
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29152
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.366
_diffrn_reflns_theta_min         3.329
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.102
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.791
_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    1.171
_exptl_crystal_description       block
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.096
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     746
_refine_ls_number_reflns         7859
_refine_ls_number_restraints     1835
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0562
_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^)+(0.0449P)^2^+3.0843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1457
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7001
_reflns_number_total             7859
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02111k2.cif
_cod_data_source_block           hasj210324a
_cod_original_cell_volume        2023.95(13)
_cod_database_code               7710812
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C86H112Al2N4Rb2
_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
 C57-C51 \\sim C51A-C57A \\sim C30-C36 \\sim C36A-C30A \\sim C44-C50 \\sim
C44A-C50A \\sim C37-C43 ~
 C37A-C43A
 with sigma of 0.02
 Al1-N2 \\sim Al1A-N2 \\sim Al1-N1 \\sim Al1A-N1
 with sigma of 0.02
 C42-C43 \\sim C43-C38
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C51A \\sim C52A \\sim C53A \\sim C54A \\sim C55A \\sim C56A \\sim C57A \\sim
C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C44A \\sim C45A \\sim C46A \\sim C47A \\sim C48A \\sim C49A \\sim C50A \\sim
C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50: within 4A with
sigma of 0.02 and sigma for terminal atoms of 0.04 within 4A
C30A \\sim C31A \\sim C32A \\sim C33A \\sim C34A \\sim C35A \\sim C36A \\sim
C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36: within 4A with
sigma of 0.02 and sigma for terminal atoms of 0.04 within 4A
Al1 \\sim Al1A: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 2A
C37A \\sim C38A \\sim C39A \\sim C40A \\sim C41A \\sim C42A \\sim C43A \\sim
C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43: within 4A with
sigma of 0.02 and sigma for terminal atoms of 0.04 within 4A
Uanis(C36) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(Rb1A)=Sof(Al1A)=1-FVAR(1)
 Sof(Rb1)=Sof(Al1)=FVAR(1)
 Sof(C51A)=Sof(C52A)=Sof(H52A)=Sof(C53A)=Sof(H53A)=Sof(C54A)=Sof(H54A)=
 Sof(C55A)=Sof(H55A)=Sof(C56A)=Sof(H56A)=Sof(C57A)=Sof(H57a)=Sof(H57b)=
 Sof(H57c)=0.5*(1-FVAR(3))
 Sof(C51)=Sof(C56)=Sof(H56)=Sof(C55)=Sof(H55)=Sof(C54)=Sof(H54)=Sof(C53)=
 Sof(H53)=Sof(C52)=Sof(H52)=Sof(C57)=Sof(H57d)=Sof(H57e)=Sof(H57f)=0.5*FVAR(3)
 Sof(C44)=Sof(C49)=Sof(H49)=Sof(C48)=Sof(H48)=Sof(C47)=Sof(H47)=Sof(C46)=
 Sof(H46)=Sof(C45)=Sof(H45)=Sof(C50)=Sof(H50d)=Sof(H50e)=Sof(H50f)=0.5*(1-
 FVAR(4))
 Sof(C44A)=Sof(C49A)=Sof(H49A)=Sof(C48A)=Sof(H48A)=Sof(C47A)=Sof(H47A)=
 Sof(C46A)=Sof(H46A)=Sof(C45A)=Sof(H45A)=Sof(C50A)=Sof(H50a)=Sof(H50b)=
 Sof(H50c)=0.5*FVAR(4)
 Sof(C30A)=Sof(C35A)=Sof(H35A)=Sof(C34A)=Sof(H34A)=Sof(C33A)=Sof(H33A)=
 Sof(C32A)=Sof(H32A)=Sof(C31A)=Sof(H31A)=Sof(C36A)=Sof(H36a)=Sof(H36b)=
 Sof(H36c)=0.5*(1-FVAR(5))
 Sof(C30)=Sof(C35)=Sof(H35)=Sof(C34)=Sof(H34)=Sof(C33)=Sof(H33)=Sof(C32)=
 Sof(H32)=Sof(C31)=Sof(H31)=Sof(C36)=Sof(H36d)=Sof(H36e)=Sof(H36f)=0.5*FVAR(5)
 Sof(C37A)=Sof(C42A)=Sof(H42A)=Sof(C41A)=Sof(H41A)=Sof(C40A)=Sof(H40A)=
 Sof(C39A)=Sof(H39A)=Sof(C38A)=Sof(H38A)=Sof(C43A)=Sof(H43a)=Sof(H43b)=
 Sof(H43c)=0.5*(1-FVAR(6))
 Sof(C37)=Sof(C42)=Sof(H42)=Sof(C41)=Sof(H41)=Sof(C40)=Sof(H40)=Sof(C39)=
 Sof(H39)=Sof(C38)=Sof(H38)=Sof(C43)=Sof(H43d)=Sof(H43e)=Sof(H43f)=0.5*FVAR(6)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C35A(H35A),
 C34A(H34A), C33A(H33A), C32A(H32A), C31A(H31A), C42A(H42A), C41A(H41A),
 C40A(H40A), C39A(H39A), C38A(H38A), C49A(H49A), C48A(H48A), C47A(H47A),
 C46A(H46A), C45A(H45A), C52A(H52A), C53A(H53A), C54A(H54A), C55A(H55A),
 C56A(H56A), C35(H35), C34(H34), C33(H33), C32(H32), C31(H31), C42(H42),
 C41(H41), C40(H40), C39(H39), C38(H38), C49(H49), C48(H48), C47(H47), C46(H46),
  C45(H45), C56(H56), C55(H55), C54(H54), C53(H53), C52(H52)
5.c Fitted hexagon refined as free rotating group:
 C30A(C35A,C34A,C33A,C32A,C31A), C37A(C42A,C41A,C40A,C39A,C38A), C44A(C49A,
 C48A,C47A,C46A,C45A), C51A(C52A,C53A,C54A,C55A,C56A), C30(C35,C34,C33,C32,C31),
  C37(C42,C41,C40,C39,C38), C44(C49,C48,C47,C46,C45), C51(C56,C55,C54,C53,C52)
5.d X=CH2 refined with riding coordinates:
 C1(H1a,H1b)
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), C36A(H36a,H36b,H36c), C43A(H43a,H43b,H43c),
 C50A(H50a,H50b,H50c), C57A(H57a,H57b,H57c), C36(H36d,H36e,H36f), C43(H43d,H43e,
 H43f), C50(H50d,H50e,H50f), C57(H57d,H57e,H57f)
;
_shelx_res_checksum              6565
_olex2_date_sample_data_collection 2021-03-24
_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 1.905
_oxdiff_exptl_absorpt_empirical_full_min 0.835