Exposing elusive cationic magnesium-chloro aggregates in aluminate complexes through donor control.
Brouillet, Etienne V.; Kennedy, Alan R.; Koszinowski, Konrad; McLellan, Ross; Mulvey, Robert E.; Robertson, Stuart D.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 5590–5597; doi:10.1039/c6dt00531d

data_7038501
_publ_section_title
;
 Exposing elusive cationic magnesium-chloro aggregates in aluminate
 complexes through donor control.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5590
_journal_page_last               5597
_journal_paper_doi               10.1039/c6dt00531d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C15 H26 Al Cl3 N Si, C12 H30 Cl Mg N4'
_chemical_formula_sum            'C27 H56 Al Cl4 Mg N5 Si'
_chemical_formula_weight         671.96
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-03-16
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;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-12-22 deposited with the CCDC.
2016-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.337(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4285(12)
_cell_length_b                   13.2180(7)
_cell_length_c                   17.5260(12)
_cell_measurement_reflns_used    5255
_cell_measurement_temperature    123.3
_cell_measurement_theta_max      28.6663
_cell_measurement_theta_min      2.9868
_cell_volume                     3678.7(5)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      123.3
_diffrn_detector_area_resol_mean 16.0727
_diffrn_measured_fraction_theta_full 0.9981
_diffrn_measured_fraction_theta_max 0.9981
_diffrn_measurement_details
;
  1 omega   34.00   71.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1756   77.0000 -120.0000 37

  2 omega   -6.00   87.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1756   77.0000  120.0000 93

  3 omega  -32.00   49.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.0350   77.0000    0.0000 81

  4 omega   34.00   93.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1756  179.0000   30.0000 59

  5 omega   -9.00   90.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1756   37.0000  -30.0000 99

  6 omega   34.00   93.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1756  179.0000 -180.0000 59

  7 omega   -6.00   19.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1756   45.0000   91.0000 25

  8 omega  -55.00   43.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1756  -37.0000  150.0000 98
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
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_diffrn_orient_matrix_UB_11      0.0234018000
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_diffrn_orient_matrix_UB_21      -0.0179377000
_diffrn_orient_matrix_UB_22      -0.0491231000
_diffrn_orient_matrix_UB_23      -0.0070802000
_diffrn_orient_matrix_UB_31      -0.0335396000
_diffrn_orient_matrix_UB_32      0.0174634000
_diffrn_orient_matrix_UB_33      -0.0369858000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1136
_diffrn_reflns_av_unetI/netI     0.1312
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40914
_diffrn_reflns_theta_full        25.9973
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.99
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.420
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.2132
_exptl_crystal_description       plate
_exptl_crystal_F_000             1443.3940
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.7940
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    80
_refine_ls_number_parameters     364
_refine_ls_number_reflns         7220
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0224
_refine_ls_R_factor_all          0.1138
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+0.7623P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.1135
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_reflns_limit_l_min              -11
_reflns_number_gt                4509
_reflns_number_total             7220
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6dt00531d2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7038500--7038504.cif.'
_cod_database_code               7038501
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.00
_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.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C16(H16a,H16b), C17(H17a,H17b), C20(H20a,H20b), C21(H21a,H21b), C24(H24a,
 H24b), C25(H25a,H25b)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5)
2.d Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C9(H9a,H9b,H9c), C11(H11a,H11b,H11c), C12(H12a,H12b,H12c),
 C13(H13a,H13b,H13c), C14(H14a,H14b,H14c), C15(H15a,H15b,H15c), C18(H18a,H18b,
 H18c), C19(H19a,H19b,H19c), C22(H22a,H22b,H22c), C23(H23a,H23b,H23c), C26(H26a,
 H26b,H26c), C27(H27a,H27b,H27c)
;
_olex2_date_sample_data_collection 2015-02-20
_olex2_date_sample_submission    2015-02-20
_olex2_submission_original_sample_id EVB043
_olex2_submission_special_instructions 'No special instructions were received'