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_7038503
_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         ' C30 H60 Cl5 Mg3 O6, C15 H26 Al Cl3 N Si'
_chemical_formula_sum            'C45 H86 Al Cl8 Mg3 N O6 Si'
_chemical_formula_weight         1148.74
_chemical_name_systematic
;
 ?
;
_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_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-10
_audit_creation_method
;
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                 95.436(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3260(3)
_cell_length_b                   14.1674(3)
_cell_length_c                   32.6193(8)
_cell_measurement_reflns_used    17679
_cell_measurement_temperature    123.3
_cell_measurement_theta_max      29.5326
_cell_measurement_theta_min      3.1312
_cell_volume                     6130.7(2)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.3
_diffrn_detector_area_resol_mean 16.0727
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
  1 omega   -8.00   84.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4192   77.0000   90.0000 92

  2 omega  -45.00   48.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4192  -77.0000  -30.0000 93

  3 omega   25.00   50.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2005   77.0000  -30.0000 25

  4 omega  -11.00   90.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4192   77.0000 -120.0000 101

  5 omega   34.00   80.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4192  179.0000  -30.0000 46

  6 omega  -46.00   52.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2005   37.0000  150.0000 98
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0061568000
_diffrn_orient_matrix_UB_12      -0.0486266000
_diffrn_orient_matrix_UB_13      -0.0047480000
_diffrn_orient_matrix_UB_21      0.0158106000
_diffrn_orient_matrix_UB_22      -0.0116275000
_diffrn_orient_matrix_UB_23      0.0207699000
_diffrn_orient_matrix_UB_31      -0.0506795000
_diffrn_orient_matrix_UB_32      0.0022815000
_diffrn_orient_matrix_UB_33      0.0048845000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            57615
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.997
_diffrn_reflns_theta_min         3.138
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95436
_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    1.245
_exptl_crystal_description       plate
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.970
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         14559
_refine_ls_number_restraints     484
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0651
_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^)+(0.0523P)^2^+11.5380P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1431
_refine_ls_wR_factor_ref         0.1620
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10691
_reflns_number_total             14559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00531d2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7038500--7038504.cif.'
_cod_database_code               7038503
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_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
 C100-C101 = C101-C23B = C23B-C102 = C102-C103 = C107-C106 = C106-C105
 1.53 with sigma of 0.01
 O2-C102 = O2-C100 = O2-C21 = O2-C24 = O3-C26 = O3-C29 = O3B-C107 = O3B-C104
 1.43 with sigma of 0.01
 C21-C22 = C22-C23 = C23-C24 = C24-C25 = C26-C27 = C27-C28 = C28-C29 = C29-C30
 1.53 with sigma of 0.01
 C105-C104 = C107-C27B = C34-C33 = C33-C32 = C32-C31 = C35-C34 = C111-C112
 1.53 with sigma of 0.01
 C111-C110 = C110-C109 = C109-C108 = C39-C38 = C38-C37 = C37-C36 = C36-C40
 1.53 with sigma of 0.01
 C113-C114 = C114-C115 = C115-C116 = C116-C117 = C41-C42 = C42-C43
 1.53 with sigma of 0.01
 C43-C44 = C44-C45 = C121-C122 = C121-C120 = C120-C119 = C119-C118
 1.53 with sigma of 0.01
 O4-C34 = O4-C31 = O4-C111 = O4-C108 = O5-C39 = O5-C36 = O5-C116 = O5-C113
 1.43 with sigma of 0.01
 O6-C41 = O6-C44 = O6-C121 = O6-C118
 1.43 with sigma of 0.01
3. Rigid bond restraints
 O2, C21, C22, C23, C24, C25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O2, C100, C101, C102, C103, C23B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O3, C26, C27, C28, C29, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C104, C105, C106, C107, O3B, C27B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4, C108, C109, C110, C111, C112
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4, C31, C32, C33, C34, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O5, C36, C37, C38, C39, C40
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O5, C113, C114, C115, C116, C117
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O6, C41, C42, C43, C44, C45
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C120, O6, C118, C119, C121, C122
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O2 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.02
O2 \\sim C100 \\sim C101 \\sim C102 \\sim C103 \\sim C23B: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.02
O3 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.02
C104 \\sim C105 \\sim C106 \\sim C107 \\sim O3B \\sim C27B: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.02
O4 \\sim C108 \\sim C109 \\sim C110 \\sim C111 \\sim C112: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.02
O4 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.02
O5 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.02
O5 \\sim C113 \\sim C114 \\sim C115 \\sim C116 \\sim C117: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.02
O6 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.02
C120 \\sim O6 \\sim C118 \\sim C119 \\sim C121 \\sim C122: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C23) = Uanis(C23B)
Uanis(O3) = Uanis(O3B)
5. Others
 Sof(C100)=Sof(H10A)=Sof(H10B)=Sof(C101)=Sof(H10C)=Sof(H10D)=Sof(C102)=
 Sof(H102)=Sof(C103)=Sof(H10E)=Sof(H10F)=Sof(H10G)=Sof(C23B)=Sof(H23C)=
 Sof(H23D)=1-FVAR(1)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=
 Sof(H23B)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1)
 Sof(C104)=Sof(H10H)=Sof(H10I)=Sof(C105)=Sof(H10J)=Sof(H10K)=Sof(C106)=
 Sof(H10L)=Sof(H10M)=Sof(C107)=Sof(H107)=Sof(O3B)=Sof(C27B)=Sof(H27C)=Sof(H27D)=
 Sof(H27E)=1-FVAR(2)
 Sof(O3)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C28)=
 Sof(H28A)=Sof(H28B)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=
 FVAR(2)
 Sof(C108)=Sof(H10N)=Sof(H10O)=Sof(C109)=Sof(H10P)=Sof(H10Q)=Sof(C110)=
 Sof(H11D)=Sof(H11E)=Sof(C111)=Sof(H111)=Sof(C112)=Sof(H1)=Sof(H2)=Sof(H11F)=1-
 FVAR(3)
 Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C33)=Sof(H33A)=
 Sof(H33B)=Sof(C34)=Sof(H34)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(3)
 Sof(C113)=Sof(H11G)=Sof(H11H)=Sof(C114)=Sof(H11I)=Sof(H11J)=Sof(C115)=
 Sof(H11K)=Sof(H11L)=Sof(C116)=Sof(H116)=Sof(C117)=Sof(H11M)=Sof(H11N)=
 Sof(H11O)=1-FVAR(4)
 Sof(C36)=Sof(H36)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(4)
 Sof(C120)=Sof(H12A)=Sof(H12B)=Sof(C118)=Sof(H11P)=Sof(H11Q)=Sof(C119)=
 Sof(H11R)=Sof(H11S)=Sof(C121)=Sof(H121)=Sof(C122)=Sof(H12D)=Sof(H12E)=
 Sof(H12F)=1-FVAR(5)
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=
 Sof(H43B)=Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=FVAR(5)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C16(H16), C24(H24), C29(H29), C34(H34), C36(H36), C44(H44),
 C102(H102), C107(H107), C111(H111), C116(H116), C121(H121)
6.b Secondary CH2 refined with riding coordinates:
 C120(H12A,H12B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C26(H26A,H26B), C27(H27A,H27B),
 C28(H28A,H28B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C37(H37A,H37B),
  C38(H38A,H38B), C39(H39A,H39B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,
 H43B), C100(H10A,H10B), C101(H10C,H10D), C104(H10H,H10I), C105(H10J,H10K),
 C106(H10L,H10M), C108(H10N,H10O), C109(H10P,H10Q), C110(H11D,H11E), C113(H11G,
 H11H), C114(H11I,H11J), C115(H11K,H11L), C118(H11P,H11Q), C119(H11R,H11S),
 C23B(H23C,H23D)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5)
6.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H6,H8,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C20(H20A,H20B,
 H20C), C25(H25A,H25B,H25C), C30(H30A,H30B,H30C), C35(H35A,H35B,H35C), C40(H40A,
 H40B,H40C), C45(H45A,H45B,H45C), C103(H10E,H10F,H10G), C112(H1,H2,H11F),
 C117(H11M,H11N,H11O), C122(H12D,H12E,H12F), C27B(H27C,H27D,H27E)
;
_olex2_submission_original_sample_id rmevb041
_olex2_submission_special_instructions 'No special instructions were received'