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_7047266
_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         'C47 H56 Mg N2 P, Al C16 F36 O4'
_chemical_formula_sum            'C66.5 H60 Al F36 Mg N2 O4 P'
_chemical_formula_weight         1717.42
_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             2018-02-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-07-04 deposited with the CCDC.
2018-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                98.276(2)
_cell_angle_beta                 93.426(2)
_cell_angle_gamma                100.177(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8232(3)
_cell_length_b                   18.2376(6)
_cell_length_c                   19.4282(4)
_cell_measurement_reflns_used    13153
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      69.8410
_cell_measurement_theta_min      4.1580
_cell_volume                     3720.96(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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 0.977
_diffrn_measured_fraction_theta_max 0.999
_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  0.0502
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            48476
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         3.119
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.785
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84166
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (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    1.533
_exptl_crystal_description       plate
_exptl_crystal_F_000             1738
_exptl_crystal_size_max          0.229
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1512
_refine_ls_number_reflns         13135
_refine_ls_number_restraints     3101
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.1027
_refine_ls_R_factor_gt           0.0904
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1821P)^2^+2.8459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2642
_refine_ls_wR_factor_ref         0.2780
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10665
_reflns_number_total             13135
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03124j2.cif
_cod_data_source_block           s18msh23
_cod_depositor_comments
'Adding full bibliography for 7047260--7047266.cif.'
_cod_original_cell_volume        3720.95(17)
_cod_original_formula_sum        'C66.50 H60 Al F36 Mg N2 O4 P'
_cod_database_code               7047266
_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
 O1_5-C1_5
 O1_6-C1_6
 O1_7-C1_7
 O1_8-C1_8
 1.35 with sigma of 0.02
 C3_3-C4_3 \\sim C2_3-C4_3 \\sim C1_3-C4_3
 with sigma of 0.005
 C1_5-C2_5 \\sim C1_5-C3_5 \\sim C1_5-C4_5
 C1_6-C2_6 \\sim C1_6-C3_6 \\sim C1_6-C4_6
 C1_7-C2_7 \\sim C1_7-C3_7 \\sim C1_7-C4_7
 C1_8-C2_8 \\sim C1_8-C3_8 \\sim C1_8-C4_8
 with sigma of 0.02
 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
 F1_6-C2_6 \\sim F2_6-C2_6 \\sim F3_6-C2_6 \\sim F4_6-C3_6 \\sim F5_6-C3_6
\\sim F6_6-C3_6 \\sim F7_6-
 C4_6 \\sim F8_6-C4_6 \\sim F9_6-C4_6
 F1_7-C2_7 \\sim F2_7-C2_7 \\sim F3_7-C2_7 \\sim F4_7-C3_7 \\sim F5_7-C3_7
\\sim F6_7-C3_7 \\sim F7_7-
 C4_7 \\sim F8_7-C4_7 \\sim F9_7-C4_7
 F1_8-C2_8 \\sim F2_8-C2_8 \\sim F3_8-C2_8 \\sim F4_8-C3_8 \\sim F5_8-C3_8
\\sim F6_8-C3_8 \\sim F7_8-
 C4_8 \\sim F8_8-C4_8 \\sim F9_8-C4_8
 with sigma of 0.02
 C2_5-C3_5 \\sim C3_5-C4_5 \\sim C2_5-C4_5
 C2_6-C3_6 \\sim C3_6-C4_6 \\sim C2_6-C4_6
 C2_7-C3_7 \\sim C3_7-C4_7 \\sim C2_7-C4_7
 C2_8-C3_8 \\sim C3_8-C4_8 \\sim C2_8-C4_8
 with sigma of 0.04
 O1_5-C2_5 \\sim O1_5-C3_5 \\sim O1_5-C4_5
 O1_6-C2_6 \\sim O1_6-C3_6 \\sim O1_6-C4_6
 O1_7-C2_7 \\sim O1_7-C3_7 \\sim O1_7-C4_7
 O1_8-C2_8 \\sim O1_8-C3_8 \\sim O1_8-C4_8
 with sigma of 0.04
 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
 F1_6-F2_6 \\sim F2_6-F3_6 \\sim F3_6-F1_6 \\sim F4_6-F5_6 \\sim F5_6-F6_6
\\sim F6_6-F4_6 \\sim F7_6-
 F8_6 \\sim F8_6-F9_6 \\sim F9_6-F7_6
 F1_7-F2_7 \\sim F2_7-F3_7 \\sim F3_7-F1_7 \\sim F4_7-F5_7 \\sim F5_7-F6_7
\\sim F6_7-F4_7 \\sim F7_7-
 F8_7 \\sim F8_7-F9_7 \\sim F9_7-F7_7
 F1_8-F2_8 \\sim F2_8-F3_8 \\sim F3_8-F1_8 \\sim F4_8-F5_8 \\sim F5_8-F6_8
\\sim F6_8-F4_8 \\sim F7_8-
 F8_8 \\sim F8_8-F9_8 \\sim F9_8-F7_8
 with sigma of 0.04
 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
 F1_6-C1_6 \\sim F2_6-C1_6 \\sim F3_6-C1_6 \\sim F4_6-C1_6 \\sim F5_6-C1_6
\\sim F6_6-C1_6 \\sim F7_6-
 C1_6 \\sim F8_6-C1_6 \\sim F9_6-C1_6
 F1_7-C1_7 \\sim F2_7-C1_7 \\sim F3_7-C1_7 \\sim F4_7-C1_7 \\sim F5_7-C1_7
\\sim F6_7-C1_7 \\sim F7_7-
 C1_7 \\sim F8_7-C1_7 \\sim F9_7-C1_7
 F1_8-C1_8 \\sim F2_8-C1_8 \\sim F3_8-C1_8 \\sim F4_8-C1_8 \\sim F5_8-C1_8
\\sim F6_8-C1_8 \\sim F7_8-
 C1_8 \\sim F8_8-C1_8 \\sim F9_8-C1_8
 with sigma of 0.1
 Al1-O1_3 \\sim Al1-O1_7 \\sim Al1-O1_4 \\sim Al1-O1_6 \\sim Al1-O1_8 \\sim
Al1-O1_1 \\sim Al1-O1_2 ~
 Al1-O1_5
 with sigma of 0.005
 O1_4-C1_4 \\sim O1_6-C1_6 \\sim O1_2-C4_2 \\sim O1_5-C1_5 \\sim O1_3-C4_3
\\sim O1_7-C1_7 \\sim O1_1-
 C4_1 \\sim O1_8-C1_8
 with sigma of 0.005
 C29A-C27 \\sim C29-C27
 with sigma of 0.005
 P1-C42 \\sim P1-C42A
 with sigma of 0.005
3. Restrained planarity
 C42, C43, C44, C45, C46, C47
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
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 \\sim
O1_6 \\sim C1_6 \\sim C2_6 \\sim F1_6 \\sim F2_6 \\sim F3_6 \\sim C3_6 \\sim
F4_6 \\sim F5_6 \\sim F6_6 \\sim C4_6 \\sim F7_6 \\sim F8_6 \\sim F9_6 \\sim
O1_7 \\sim C1_7 \\sim C2_7 \\sim F1_7 \\sim F2_7 \\sim F3_7 \\sim C3_7 \\sim
F4_7 \\sim F5_7 \\sim F6_7 \\sim C4_7 \\sim F7_7 \\sim F8_7 \\sim F9_7 \\sim
O1_8 \\sim C1_8 \\sim C2_8 \\sim F1_8 \\sim F2_8 \\sim F3_8 \\sim C3_8 \\sim
F4_8 \\sim F5_8 \\sim F6_8 \\sim C4_8 \\sim F7_8 \\sim F8_8 \\sim F9_8: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C42A \\sim C47A \\sim C46A \\sim C45A \\sim C44A \\sim C43A: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.01
C43 \\sim C42 \\sim C47 \\sim C46 \\sim C45 \\sim C44: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.01
Uanis(F2_4) = Uanis(F9_6)
Uanis(C4_1) = Uanis(C1_8)
Uanis(O1_1) = Uanis(O1_8)
5. Rigid body (RIGU) restrains
 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_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
 O1_6, C1_6, C2_6, F1_6, F2_6, F3_6, C3_6, F4_6, F5_6, F6_6, C4_6, F7_6, F8_6,
 F9_6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1_7, C1_7, C2_7, F1_7, F2_7, F3_7, C3_7, F4_7, F5_7, F6_7, C4_7, F7_7, F8_7,
 F9_7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1_8, C1_8, C2_8, F1_8, F2_8, F3_8, C3_8, F4_8, F5_8, F6_8, C4_8, F7_8, F8_8,
 F9_8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: H27(0.65) H27A(0.35) C42(0.65) C47(0.65) H47(0.65) C46(0.65)
 H46(0.65) C45(0.65) H45(0.65) C44(0.65) H44(0.65) C43(0.65) H43(0.65)
 C29(0.65) H29A(0.65) H29B(0.65) H29C(0.65) C29A(0.35) H29D(0.35) H29E(0.35)
 H29F(0.35) C42A(0.35) C47A(0.35) H47A(0.35) C46A(0.35) H46A(0.35) C45A(0.35)
 H45A(0.35) C44A(0.35) H44A(0.35) C43A(0.35) H43A(0.35) F1(0.75) F2(0.75)
 F3(0.75) F4(0.75) F5(0.75) F6(0.75) F7(0.75) F8(0.75) F9(0.75) O1(0.75)
 C1(0.75) C2(0.75) C3(0.75) C4(0.75) F1(0.65) F2(0.65) F3(0.65) F4(0.65)
 F5(0.65) F6(0.65) F7(0.65) F8(0.65) F9(0.65) O1(0.65) C1(0.65) C2(0.65)
 C3(0.65) C4(0.65) F1(0.55) F2(0.55) F3(0.55) F4(0.55) F5(0.55) F6(0.55)
 F7(0.55) F8(0.55) F9(0.55) O1(0.55) C1(0.55) C2(0.55) C3(0.55) C4(0.55)
 F1(0.65) F2(0.65) F3(0.65) F4(0.65) F5(0.65) F6(0.65) F7(0.65) F8(0.65)
 F9(0.65) O1(0.65) C1(0.65) C2(0.65) C3(0.65) C4(0.65) O1(0.35) C1(0.35)
 C2(0.35) F1(0.35) F2(0.35) F3(0.35) C3(0.35) F4(0.35) F5(0.35) F6(0.35)
 C4(0.35) F7(0.35) F8(0.35) F9(0.35) O1(0.35) C1(0.35) C2(0.35) F1(0.35)
 F2(0.35) F3(0.35) C3(0.35) F4(0.35) F5(0.35) F6(0.35) C4(0.35) F7(0.35)
 F8(0.35) F9(0.35) O1(0.45) C1(0.45) C2(0.45) F1(0.45) F2(0.45) F3(0.45)
 C3(0.45) F4(0.45) F5(0.45) F6(0.45) C4(0.45) F7(0.45) F8(0.45) F9(0.45)
 O1(0.25) C1(0.25) C2(0.25) F1(0.25) F2(0.25) F3(0.25) C3(0.25) F4(0.25)
 F5(0.25) F6(0.25) C4(0.25) F7(0.25) F8(0.25) F9(0.25)
7.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C27(H27A)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C31(H31),
 C32(H32), C33(H33), C34(H34), C35(H35), C37(H37), C38(H38), C39(H39), C40(H40),
  C41(H41), C47(H47), C46(H46), C45(H45), C44(H44), C43(H43), C47A(H47A),
 C46A(H46A), C45A(H45A), C44A(H44A), C43A(H43A)
7.c Fitted hexagon refined as free rotating group:
 C42(C47,C46,C45,C44,C43), C42A(C47A,C46A,C45A,C44A,C43A)
7.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), 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), C29A(H29D,H29E,H29F)
;
_olex2_submission_special_instructions 'No special instructions were received'