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_7047262
_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 H53 F6 Mg N2, Al C16 F36 O4, C6 H4 F2'
_chemical_formula_sum            'C69 H57 Al F44 Mg N2 O4'
_chemical_formula_weight         1865.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_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     iterative
_audit_creation_date             2018-06-07
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-07 deposited with the CCDC.
2018-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.0273(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.3502(3)
_cell_length_b                   21.2981(3)
_cell_length_c                   19.3981(4)
_cell_measurement_reflns_used    15368
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.8360
_cell_measurement_theta_min      3.7020
_cell_volume                     7818.9(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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_temperature      150.15
_diffrn_detector_area_resol_mean 16.1468
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            62004
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.314
_exptl_absorpt_coefficient_mu    0.187
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.956
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_description       block
_exptl_crystal_F_000             3752
_exptl_crystal_size_max          0.385
_exptl_crystal_size_mid          0.3555
_exptl_crystal_size_min          0.1976
_refine_diff_density_max         1.043
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1178
_refine_ls_number_reflns         15646
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1373
_refine_ls_R_factor_gt           0.0835
_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^)+(0.1136P)^2^+14.5032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2148
_refine_ls_wR_factor_ref         0.2543
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9420
_reflns_number_total             15646
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03124j2.cif
_cod_data_source_block           e14msh7
_cod_depositor_comments
'Adding full bibliography for 7047260--7047266.cif.'
_cod_database_code               7047262
_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
 Mg1-F5 \\sim Mg1-F5A
 with sigma of 0.005
 F5-C42 \\sim F5A-C42A
 with sigma of 0.005
3. Restrained planarity
 C46, C44, F6, C43, F5, C45, C47, C42
 with sigma of 0.1
 F5A, F6A, C42A, C43A, C44A, C45A, C46A, C47A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C46 \\sim C44 \\sim F6 \\sim C43 \\sim F5 \\sim C45 \\sim C47: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01
F5A \\sim F6A \\sim C43A \\sim C44A \\sim C45A \\sim C46A \\sim C47A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
O4 \\sim O4A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C42) = Uanis(C42A)
5. Others
 Fixed Sof: F5A(0.5) F6A(0.5) C42A(0.5) C47A(0.5) H47A(0.5) C46A(0.5)
 H46A(0.5) C45A(0.5) C44A(0.5) H44A(0.5) C43A(0.5) H43A(0.5) O4(0.6) O4A(0.4)
 O3(0.6) O3A(0.4) F43(0.65) H64(0.35) H65(0.65) H67(0.35) H68(0.65) F6(0.5)
 F5(0.5) F43A(0.35) F44(0.65) F44A(0.35) C42(0.5) C47(0.5) H47(0.5) C46(0.5)
 H46(0.5) C45(0.5) C44(0.5) H44(0.5) C43(0.5) H43(0.5)
6.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27)
6.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), C34(H34), C35(H35), C37(H37), C38(H38), C40(H40), C41(H41),
 C47A(H47A), C46A(H46A), C44A(H44A), C43A(H43A), C64(H64), C65(H65), C66(H66),
 C67(H67), C68(H68), C69(H69), C47(H47), C46(H46), C44(H44), C43(H43)
6.c Fitted hexagon refined as free rotating group:
 C42A(C47A,C46A,C45A,C44A,C43A), C42(C47,C46,C45,C44,C43)
6.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)
;
_olex2_submission_special_instructions 'No special instructions were received'