Synthesis of magnesium complexes of ionic liquids with highly coordinating anions.
Lethesh, Kallidanthiyil Chellappan; Øien-Ødegaard, Sigurd; Jayasayee, Kaushik; Fiksdahl, Anne; Dalton transactions (Cambridge, England : 2003) 48 (2019) 982–988; doi:10.1039/c8dt04364g

data_7048348
_publ_section_title
;
 Synthesis of magnesium complexes of ionic liquids with highly
 coordinating anions.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              982
_journal_page_last               988
_journal_paper_doi               10.1039/c8dt04364g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C15 H3 F18 Mg O6, C10 H22 N'
_chemical_formula_sum            'C25 H25 F18 Mg N O6'
_chemical_formula_weight         801.77
_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
_audit_creation_date             2018-07-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-31 deposited with the CCDC.
2018-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.444(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.549(2)
_cell_length_b                   18.597(2)
_cell_length_c                   20.171(2)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.297
_cell_measurement_theta_min      2.329
_cell_volume                     6476.4(12)
_computing_cell_refinement       'APEX3 (Bruker AXS, 2016)'
_computing_data_collection       'APEX3 (Bruker AXS, 2016)'
_computing_data_reduction        'APEX3 (Bruker AXS, 2016)'
_computing_molecular_graphics    'Diamond v4 (Brandenburg, 2012)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture, CMOS detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            54735
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.329
_diffrn_reflns_theta_min         2.190
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0882 before and 0.0422 after correction. The Ratio of minimum to maximum transmission is 0.9114. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_description       block
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.191
_exptl_crystal_size_min          0.089
_refine_diff_density_max         1.325
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1082
_refine_ls_number_reflns         16076
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0663
_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^)+(0.1136P)^2^+8.1300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1783
_refine_ls_wR_factor_ref         0.2035
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11802
_reflns_number_total             16076
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04364g2.cif
_cod_data_source_block           kcl-105-first_pl
_cod_depositor_comments
'Adding full bibliography for 7048346--7048349.cif.'
_cod_database_code               7048348
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.948
_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
 F33-F31
 2.15 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
Uanis(F11) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F10)
\\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F31) \\sim Ueq, Uanis(F5) \\sim Ueq,
Uanis(F14) \\sim Ueq, Uanis(F33) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(F34) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
4. Others
 Sof(F31)=Sof(F32)=Sof(F33)=1-FVAR(1)
 Sof(F28)=Sof(F29)=Sof(F30)=FVAR(1)
 Sof(F10)=Sof(F11)=Sof(F12)=1-FVAR(2)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(2)
 Sof(F16)=Sof(F17)=Sof(F18)=1-FVAR(3)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(3)
 Sof(F4)=Sof(F5)=Sof(F6)=1-FVAR(4)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(4)
 Sof(N3)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(C56)=
 Sof(H56A)=Sof(H56B)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(C53)=Sof(H53A)=Sof(H53B)=
 Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(C57)=
 Sof(H57A)=Sof(H57B)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(C59)=Sof(H59A)=Sof(H59B)=
 Sof(H59C)=1-FVAR(5)
 Sof(N1)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C40)=
 Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C34)=Sof(H34A)=
 Sof(H34B)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C35)=
 Sof(H35A)=Sof(H35B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=
 Sof(H39C)=FVAR(5)
5.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C36(H36A,H36B), C32(H32A,H32B), C34(H34A,H34B), C31(H31A,
 H31B), C33(H33A,H33B), C35(H35A,H35B), C38(H38A,H38B), C43(H43A,H43B),
 C42(H42A,H42B), C46(H46A,H46B), C41(H41A,H41B), C48(H48A,H48B), C45(H45A,H45B),
  C47(H47A,H47B), C44(H44A,H44B), C54(H54A,H54B), C50(H50A,H50B), C56(H56A,
 H56B), C51(H51A,H51B), C53(H53A,H53B), C58(H58A,H58B), C57(H57A,H57B),
 C52(H52A,H52B)
5.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C3(H3), C8(H8), C28(H28), C23(H23), C18(H18)
5.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C39(H39A,H39B,H39C), C3AA(H3AA,H3AB,H3AC), C49(H49A,H49B,
 H49C), C55(H55A,H55B,H55C), C59(H59A,H59B,H59C)
;
_olex2_submission_special_instructions 'No special instructions were received'