Structural analysis of five-coordinate aluminium(salen) complexes and its relationship to their catalytic activity.
Fish, Heather; Hart, Sam; Lamb, Katie J.; North, Michael; Quek, Sophie C. Z.; Whitwood, Adrian C.; Woods, Barnaby; Wu, Xiao; Dalton transactions (Cambridge, England : 2003) 50 (2021) 587–598; doi:10.1039/d0dt03598j

data_7706064
_publ_section_title
;
 Structural analysis of five-coordinate aluminium(salen) complexes and its
 relationship to their catalytic activity.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              587
_journal_page_last               598
_journal_paper_doi               10.1039/d0dt03598j
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'Cl, C72 H107 Al2 N4 O6, 0.313(H2 O)'
_chemical_formula_sum            'C72 H107.62 Al2 Cl N4 O6.31'
_chemical_formula_weight         1219.61
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-11-10
_audit_creation_method
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Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
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_audit_update_record
;
2020-11-10 deposited with the CCDC.	2020-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4538(4)
_cell_length_b                   19.9792(4)
_cell_length_c                   28.2756(6)
_cell_measurement_reflns_used    10929
_cell_measurement_temperature    110.1(2)
_cell_measurement_theta_max      31.3450
_cell_measurement_theta_min      3.2750
_cell_volume                     8165.3(3)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.1(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_details
;
  1 omega  -81.00  -45.00   0.7500  125.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1672  -77.0000  120.0000 48

  2 omega   44.00   88.25   0.7500  125.0000
omega____ theta____ kappa____ phi______ frames
    -       26.5735  178.0000  -90.0000 59

  3 omega  -36.00   40.50   0.7500  125.0000
omega____ theta____ kappa____ phi______ frames
    -       26.5735  -37.0000    0.0000 102

  4 omega  -95.00  -69.50   0.7500  125.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1672  -77.0000    0.0000 34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0171529000
_diffrn_orient_matrix_UB_12      -0.0244000000
_diffrn_orient_matrix_UB_13      0.0159810000
_diffrn_orient_matrix_UB_21      0.0457087000
_diffrn_orient_matrix_UB_22      -0.0113634000
_diffrn_orient_matrix_UB_23      0.0041706000
_diffrn_orient_matrix_UB_31      0.0044309000
_diffrn_orient_matrix_UB_32      0.0231941000
_diffrn_orient_matrix_UB_33      0.0188889000
_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  0.0321
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            37091
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.782
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         32.227
_diffrn_reflns_theta_min         2.867
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.965
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.992
_exptl_crystal_description       block
_exptl_crystal_F_000             2644
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane'
_exptl_crystal_size_max          0.3377
_exptl_crystal_size_mid          0.253
_exptl_crystal_size_min          0.1485
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 6207 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.14(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     808
_refine_ls_number_reflns         22588
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0773P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1322
_reflns_Friedel_coverage         0.604
_reflns_Friedel_fraction_full    0.799
_reflns_Friedel_fraction_max     0.636
_reflns_number_gt                18692
_reflns_number_total             22588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03598j2.cif
_cod_data_source_block           mn1405
_cod_depositor_comments          'Adding full bibliography for 7706064.cif.'
_cod_database_code               7706064
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C36 H52 Al1 Cl1 N2 O2'
_chemical_oxdiff_usercomment     'Sophie's SQ2002'
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.963
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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, All O(H,H) groups
2. Others
 Sof(O7)=Sof(H7A)=Sof(H7B)=FVAR(1)
3.a Free rotating group:
 O7(H7A,H7B)
3.b Rotating group:
 O3(H3A,H3B)
3.c Ternary CH refined with riding coordinates:
 C16(H16), C21(H21), C52(H52), C57(H57)
3.d Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C53(H53A,
 H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B)
3.e Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C22(H22), C24(H24), C26(H26), C39(H39), C41(H41),
 C43(H43), C58(H58), C60(H60), C62(H62)
3.f Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,
 H47C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C66(H66A,
 H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C),
 C71(H71A,H71B,H71C), C72(H72A,H72B,H72C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              4984
_shelx_fab_checksum              19618
_olex2_date_sample_data_collection 2014-04-09
_olex2_date_sample_submission    2014-03-28
_olex2_exptl_crystal_mounting_method 'oil on loop'
_olex2_submission_original_sample_id SQ2002
_olex2_submission_special_instructions 'No special instructions were received'