Coordination of arenes and phosphines by charge separated alkaline earth cations.
Garcia, Lucia; Anker, Mathew D.; Mahon, Mary F.; Maron, Laurent; Hill, Michael S.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 12684–12693; doi:10.1039/c8dt03124j

data_7047260
_publ_section_title
;
 Coordination of arenes and phosphines by charge separated alkaline earth
 cations.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12684
_journal_page_last               12693
_journal_paper_doi               10.1039/c8dt03124j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'Al C16 F36 O4, C36 H49 Mg N2, C3 H7'
_chemical_formula_sum            'C55 H56 Al F36 Mg N2 O4'
_chemical_formula_weight         1544.30
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-02-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-18 deposited with the CCDC.
2018-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                83.048(2)
_cell_angle_beta                 88.150(2)
_cell_angle_gamma                74.609(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7692(2)
_cell_length_b                   15.7438(5)
_cell_length_c                   19.8667(4)
_cell_measurement_reflns_used    20772
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.9400
_cell_measurement_theta_min      4.8140
_cell_volume                     3223.69(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            41540
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.275
_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    1.756
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_description       plate
_exptl_crystal_F_000             1562
_exptl_crystal_size_max          0.402
_exptl_crystal_size_mid          0.293
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1292
_refine_ls_number_reflns         12877
_refine_ls_number_restraints     4327
_refine_ls_restrained_S_all      1.303
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0666
_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^)+(0.1287P)^2^+2.1355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1912
_refine_ls_wR_factor_ref         0.1998
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11348
_reflns_number_total             12877
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03124j2.cif
_cod_data_source_block           s18msh17
_cod_depositor_comments
'Adding full bibliography for 7047260--7047266.cif.'
_cod_database_code               7047260
_shelxl_version_number           2014-3
_chemical_oxdiff_usercomment     'colorless plate'
_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
 C2_3-C1_3 = C2_4-C1_4 = C3_4-C1_4 = C4_3-C1_3 = C4_4-C1_4 = C3_3-C1_3
 1.54 with sigma of 0.005
 C1_1-C2_1 \\sim C1_1-C3_1 \\sim C1_1-C4_1
 C1_2-C2_2 \\sim C1_2-C3_2 \\sim C1_2-C4_2
 C1_3-C2_3 \\sim C1_3-C3_3 \\sim C1_3-C4_3
 C1_4-C2_4 \\sim C1_4-C3_4 \\sim C1_4-C4_4
 C1_5-C2_5 \\sim C1_5-C3_5 \\sim C1_5-C4_5
 with sigma of 0.02
 F1_1-C2_1 \\sim F2_1-C2_1 \\sim F3_1-C2_1 \\sim F4_1-C3_1 \\sim F5_1-C3_1
\\sim F6_1-C3_1 \\sim F7_1-
 C4_1 \\sim F8_1-C4_1 \\sim F9_1-C4_1
 F1_2-C2_2 \\sim F2_2-C2_2 \\sim F3_2-C2_2 \\sim F4_2-C3_2 \\sim F5_2-C3_2
\\sim F6_2-C3_2 \\sim F7_2-
 C4_2 \\sim F8_2-C4_2 \\sim F9_2-C4_2
 F1_3-C2_3 \\sim F2_3-C2_3 \\sim F3_3-C2_3 \\sim F4_3-C3_3 \\sim F5_3-C3_3
\\sim F6_3-C3_3 \\sim F7_3-
 C4_3 \\sim F8_3-C4_3 \\sim F9_3-C4_3
 F1_4-C2_4 \\sim F2_4-C2_4 \\sim F3_4-C2_4 \\sim F4_4-C3_4 \\sim F5_4-C3_4
\\sim F6_4-C3_4 \\sim F7_4-
 C4_4 \\sim F8_4-C4_4 \\sim F9_4-C4_4
 F1_5-C2_5 \\sim F2_5-C2_5 \\sim F3_5-C2_5 \\sim F4_5-C3_5 \\sim F5_5-C3_5
\\sim F6_5-C3_5 \\sim F7_5-
 C4_5 \\sim F8_5-C4_5 \\sim F9_5-C4_5
 with sigma of 0.02
 C2_1-C3_1 \\sim C3_1-C4_1 \\sim C2_1-C4_1
 C2_2-C3_2 \\sim C3_2-C4_2 \\sim C2_2-C4_2
 C2_3-C3_3 \\sim C3_3-C4_3 \\sim C2_3-C4_3
 C2_4-C3_4 \\sim C3_4-C4_4 \\sim C2_4-C4_4
 C2_5-C3_5 \\sim C3_5-C4_5 \\sim C2_5-C4_5
 with sigma of 0.04
 C2_1-C3_1 \\sim C4_1-?
 O1_2-C2_2 \\sim O1_2-C3_2 \\sim O1_2-C4_2
 O1_3-C2_3 \\sim O1_3-C3_3 \\sim O1_3-C4_3
 O1_4-C2_4 \\sim O1_4-C3_4 \\sim O1_4-C4_4
 O1_5-C2_5 \\sim O1_5-C3_5 \\sim O1_5-C4_5
 with sigma of 0.04
 F1_1-F2_1 \\sim F2_1-F3_1 \\sim F3_1-F1_1 \\sim F4_1-F5_1 \\sim F5_1-F6_1
\\sim F6_1-F4_1 \\sim F7_1-
 F8_1 \\sim F8_1-F9_1 \\sim F9_1-F7_1
 F1_2-F2_2 \\sim F2_2-F3_2 \\sim F3_2-F1_2 \\sim F4_2-F5_2 \\sim F5_2-F6_2
\\sim F6_2-F4_2 \\sim F7_2-
 F8_2 \\sim F8_2-F9_2 \\sim F9_2-F7_2
 F1_3-F2_3 \\sim F2_3-F3_3 \\sim F3_3-F1_3 \\sim F4_3-F5_3 \\sim F5_3-F6_3
\\sim F6_3-F4_3 \\sim F7_3-
 F8_3 \\sim F8_3-F9_3 \\sim F9_3-F7_3
 F1_4-F2_4 \\sim F2_4-F3_4 \\sim F3_4-F1_4 \\sim F4_4-F5_4 \\sim F5_4-F6_4
\\sim F6_4-F4_4 \\sim F7_4-
 F8_4 \\sim F8_4-F9_4 \\sim F9_4-F7_4
 F1_5-F2_5 \\sim F2_5-F3_5 \\sim F3_5-F1_5 \\sim F4_5-F5_5 \\sim F5_5-F6_5
\\sim F6_5-F4_5 \\sim F7_5-
 F8_5 \\sim F8_5-F9_5 \\sim F9_5-F7_5
 with sigma of 0.04
 F1_1-C1_1 \\sim F2_1-C1_1 \\sim F3_1-C1_1 \\sim F4_1-C1_1 \\sim F5_1-C1_1
\\sim F6_1-C1_1 \\sim F7_1-
 C1_1 \\sim F8_1-C1_1 \\sim F9_1-C1_1
 F1_2-C1_2 \\sim F2_2-C1_2 \\sim F3_2-C1_2 \\sim F4_2-C1_2 \\sim F5_2-C1_2
\\sim F6_2-C1_2 \\sim F7_2-
 C1_2 \\sim F8_2-C1_2 \\sim F9_2-C1_2
 F1_3-C1_3 \\sim F2_3-C1_3 \\sim F3_3-C1_3 \\sim F4_3-C1_3 \\sim F5_3-C1_3
\\sim F6_3-C1_3 \\sim F7_3-
 C1_3 \\sim F8_3-C1_3 \\sim F9_3-C1_3
 F1_4-C1_4 \\sim F2_4-C1_4 \\sim F3_4-C1_4 \\sim F4_4-C1_4 \\sim F5_4-C1_4
\\sim F6_4-C1_4 \\sim F7_4-
 C1_4 \\sim F8_4-C1_4 \\sim F9_4-C1_4
 F1_5-C1_5 \\sim F2_5-C1_5 \\sim F3_5-C1_5 \\sim F4_5-C1_5 \\sim F5_5-C1_5
\\sim F6_5-C1_5 \\sim F7_5-
 C1_5 \\sim F8_5-C1_5 \\sim F9_5-C1_5
 with sigma of 0.1
 Al1-O1_4 \\sim Al1-O1_3 \\sim Al1-O4 \\sim Al1-O2_1 \\sim Al1-O1_5 \\sim
Al1-O1_2
 with sigma of 0.01
 O1_2-C1_2 \\sim O1_5-C1_5 \\sim O2_1-C1_1 \\sim O1_3-C1_3 \\sim O1_4-C1_4
\\sim O4-C37
 with sigma of 0.01
 F6A-F4A \\sim F6A-F5A \\sim F5A-F4A
 with sigma of 0.01
 C3A-F6A \\sim C3A-F4A \\sim C3A-F5A
 with sigma of 0.01
 C4A-F8A \\sim C4A-F9A \\sim C4A-F7A
 with sigma of 0.01
 F2A-F3A \\sim F3A-F1A
 with sigma of 0.01
 C2A-F2A \\sim C2A-F3A \\sim C2A-F1A
 with sigma of 0.01
 C4A-C1_1 \\sim C4_1-C1_1 \\sim C2A-C1_1 \\sim C2_1-C1_1 \\sim C3A-C1_1 \\sim
C3_1-C1_1
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C1_1 \\sim C2_1 \\sim F1_1 \\sim F2_1 \\sim F3_1 \\sim C3_1 \\sim F4_1 \\sim
F5_1 \\sim F6_1 \\sim C4_1 \\sim F7_1 \\sim F8_1 \\sim F9_1 \\sim O1_2 \\sim
C1_2 \\sim C2_2 \\sim F1_2 \\sim F2_2 \\sim F3_2 \\sim C3_2 \\sim F4_2 \\sim
F5_2 \\sim F6_2 \\sim C4_2 \\sim F7_2 \\sim F8_2 \\sim F9_2 \\sim O1_3 \\sim
C1_3 \\sim C2_3 \\sim F1_3 \\sim F2_3 \\sim F3_3 \\sim C3_3 \\sim F4_3 \\sim
F5_3 \\sim F6_3 \\sim C4_3 \\sim F7_3 \\sim F8_3 \\sim F9_3 \\sim O1_4 \\sim
C1_4 \\sim C2_4 \\sim F1_4 \\sim F2_4 \\sim F3_4 \\sim C3_4 \\sim F4_4 \\sim
F5_4 \\sim F6_4 \\sim C4_4 \\sim F7_4 \\sim F8_4 \\sim F9_4 \\sim O1_5 \\sim
C1_5 \\sim C2_5 \\sim F1_5 \\sim F2_5 \\sim F3_5 \\sim C3_5 \\sim F4_5 \\sim
F5_5 \\sim F6_5 \\sim C4_5 \\sim F7_5 \\sim F8_5 \\sim F9_5: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C4A \\sim F8A \\sim F9A \\sim F7A \\sim F2A \\sim F3A \\sim C2A \\sim F1A \\sim
F5A \\sim F4A \\sim F6A \\sim C3A \\sim C1_1: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 F6A, C3A, F4A, C2A, F2A, F3A, F1A, F8A, C4A, F5A, F9A, F7A, C1_1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1_2, C1_2, C2_2, F1_2, F2_2, F3_2, C3_2, F4_2, F5_2, F6_2, C4_2, F7_2, F8_2,
 F9_2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1_3, C1_3, C2_3, F1_3, F2_3, F3_3, C3_3, F4_3, F5_3, F6_3, C4_3, F7_3, F8_3,
 F9_3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1_4, C1_4, C2_4, F1_4, F2_4, F3_4, C3_4, F4_4, F5_4, F6_4, C4_4, F7_4, F8_4,
 F9_4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1_5, C1_5, C2_5, F1_5, F2_5, F3_5, C3_5, F4_5, F5_5, F6_5, C4_5, F7_5, F8_5,
 F9_5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C56(0.5) H56A(0.5) H56B(0.5) C57(0.5) H57A(0.5) H57B(0.5) C58(0.5)
 H58A(0.5) H58B(0.5) H58C(0.5) F6A(0.4) C3A(0.4) F4A(0.4) C2A(0.4) F2A(0.4)
 F3A(0.4) F1A(0.4) F8A(0.4) C4A(0.4) F5A(0.4) F9A(0.4) F7A(0.4) C58A(0.5)
 H58D(0.5) H58E(0.5) H58F(0.5) C57A(0.5) H57C(0.5) H57D(0.5) C56A(0.5)
 H56C(0.5) H56D(0.5) F1(0.6) F2(0.6) F3(0.6) F4(0.6) F5(0.6) F6(0.6) F7(0.6)
 F8(0.6) F9(0.6) C2(0.6) C3(0.6) C4(0.6) F1(0.6) F2(0.6) F3(0.6) F4(0.6)
 F5(0.6) F6(0.6) F7(0.6) F8(0.6) F9(0.6) O1(0.6) C1(0.6) C2(0.6) C3(0.6)
 C4(0.6) F1(0.6) F2(0.6) F3(0.6) F4(0.6) F5(0.6) F6(0.6) F7(0.6) F8(0.6)
 F9(0.6) O1(0.6) C1(0.6) C2(0.6) C3(0.6) C4(0.6) F1(0.4) F2(0.4) F3(0.4)
 F4(0.4) F5(0.4) F6(0.4) F7(0.4) F8(0.4) F9(0.4) O1(0.4) C1(0.4) C2(0.4)
 C3(0.4) C4(0.4) F1(0.4) F2(0.4) F3(0.4) F4(0.4) F5(0.4) F6(0.4) F7(0.4)
 F8(0.4) F9(0.4) O1(0.4) C1(0.4) C2(0.4) C3(0.4) C4(0.4)
6.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27)
6.b Secondary CH2 refined with riding coordinates:
 C56(H56A,H56B), C57(H57A,H57B), C57A(H57C,H57D), C56A(H56C,H56D)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C30(H30),
 C31(H31), C33(H33), C34(H34), C35(H35)
6.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), 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), C36(H36A,H36B,H36C), C58(H58A,
 H58B,H58C), C58A(H58D,H58E,H58F)
;
_olex2_submission_special_instructions 'No special instructions were received'