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_7047265
_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         'C53 H68 Mg N2 P, Al C16 F36 O4'
_chemical_formula_sum            'C69 H68 Al F36 Mg N2 O4 P'
_chemical_formula_weight         1755.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-10-14
_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                90
_cell_angle_beta                 101.266(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5387(2)
_cell_length_b                   35.7529(6)
_cell_length_c                   16.0778(3)
_cell_measurement_reflns_used    14842
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.3520
_cell_measurement_theta_min      3.7410
_cell_volume                     7632.5(2)
_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 1.000
_diffrn_measured_fraction_theta_max 0.988
_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  0.0362
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            54773
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.181
_diffrn_reflns_theta_min         3.063
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.753
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86028
_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    1.528
_exptl_crystal_description       tabloid
_exptl_crystal_F_000             3568
_exptl_crystal_size_max          0.164
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.081
_refine_diff_density_max         1.513
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1544
_refine_ls_number_reflns         15127
_refine_ls_number_restraints     3635
_refine_ls_restrained_S_all      1.214
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0692
_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^)+(0.1044P)^2^+8.0528P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1857
_refine_ls_wR_factor_ref         0.2017
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11722
_reflns_number_total             15127
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03124j2.cif
_cod_data_source_block           s17msh108
_cod_depositor_comments
'Adding full bibliography for 7047260--7047266.cif.'
_cod_database_code               7047265
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(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
 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 0.02
 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 0.02
 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 0.02
 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
 C34-H34A \\sim C34-H34C \\sim C34-H34B
 with sigma of 0.005
 Al1-O1_2 \\sim Al1-O1_6 \\sim Al1-O1_1 \\sim Al1-O1_5 \\sim Al1-O1_3 \\sim
Al1-O1_8 \\sim Al1-O1_7 ~
 Al1-O1_4
 with sigma of 0.005
3. 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
O1_1 \\sim 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: within
2A with sigma of 0.03 and sigma for terminal atoms of 0.01
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: within
2A with sigma of 0.03 and sigma for terminal atoms of 0.01
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: within
2A with sigma of 0.03 and sigma for terminal atoms of 0.01
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: within
2A with sigma of 0.03 and sigma for terminal atoms of 0.01
Uanis(O1_5) = Uanis(O1_1)
Uanis(O1_4) = Uanis(O1_7)
4. Rigid body (RIGU) restrains
 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
 O1_1, C1_1, C2_1, F1_1, F2_1, F3_1, C3_1, F4_1, F5_1, F6_1, C4_1, F7_1, F8_1,
 F9_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
5. Others
 Fixed Sof: O1(0.65) C1(0.65) C2(0.65) F1(0.65) F2(0.65) F3(0.65) C3(0.65)
 F4(0.65) F5(0.65) F6(0.65) C4(0.65) F7(0.65) F8(0.65) F9(0.65) O1(0.65)
 C1(0.65) C2(0.65) F1(0.65) F2(0.65) F3(0.65) C3(0.65) F4(0.65) F5(0.65)
 F6(0.65) C4(0.65) F7(0.65) F8(0.65) F9(0.65) O1(0.65) C1(0.65) C2(0.65)
 F1(0.65) F2(0.65) F3(0.65) C3(0.65) F4(0.65) F5(0.65) F6(0.65) C4(0.65)
 F7(0.65) F8(0.65) F9(0.65) O1(0.65) C1(0.65) C2(0.65) F1(0.65) F2(0.65)
 F3(0.65) C3(0.65) F4(0.65) F5(0.65) F6(0.65) C4(0.65) F7(0.65) F8(0.65)
 F9(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(0.35) 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)
6.a Ternary CH refined with riding coordinates:
 C18(H18), C21(H21), C30(H30), C33(H33)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C14(H14), C15(H15), C16(H16), C26(H26), C27(H27), C28(H28), C37(H37),
 C38(H38), C39(H39), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45), C46(H46),
  C47(H47), C49(H49), C50(H50), C52(H52), C53(H53), C54(H54)
6.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C),
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C35(H35A,H35B,H35C)
;
_olex2_submission_special_instructions 'No special instructions were received'