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_7048349
_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, C8 H15 N2'
_chemical_formula_sum            'C23 H18 F18 Mg N2 O6'
_chemical_formula_weight         784.70
_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
_audit_creation_date             2018-07-11
_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                74.180(2)
_cell_angle_beta                 86.894(2)
_cell_angle_gamma                89.008(2)
_cell_formula_units_Z            4
_cell_length_a                   9.0058(8)
_cell_length_b                   17.6783(15)
_cell_length_c                   20.1473(17)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.96
_cell_measurement_theta_min      2.34
_cell_volume                     3081.6(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0610
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            77620
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.257
_diffrn_reflns_theta_min         2.265
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.208
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1156 before and 0.0532 after correction. The Ratio of minimum to maximum transmission is 0.9295. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.249
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.907
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     968
_refine_ls_number_reflns         11140
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+5.8115P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1239
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7954
_reflns_number_total             11140
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04364g2.cif
_cod_data_source_block           kcl-40_pl
_cod_depositor_comments
'Adding full bibliography for 7048346--7048349.cif.'
_cod_database_code               7048349
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.950
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C47) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(F13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F2) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(F6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F3) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 C47, C46, C45, C44, C43
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F10, F11, F12, F13, F14, F15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1, F2, F3, F4, F5, F6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: F10(0.859) F11(0.859) F12(0.859) F1(0.679) F2(0.679) F3(0.679)
 F4(0.321) F5(0.321) F6(0.321) F13(0.141) F14(0.141) F15(0.141) C45(0.835)
 H45A(0.835) H45B(0.835) H44C(0.835) H44D(0.835) H44A(0.165) H44B(0.165)
 H46D(0.835) H46E(0.835) H46F(0.835) H46A(0.165) H46B(0.165) H46C(0.165)
 C47(0.165) H47A(0.165) H47B(0.165)
5.a Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C45(H45A,H45B), C44(H44C,H44D), C44(H44A,H44B), C47(H47A,
 H47B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C13(H13), C3(H3), C23(H23), C18(H18), C28(H28), C39(H39), C40(H40),
 C41(H41), C31(H31), C32(H32), C33(H33)
5.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C46(H46D,H46E,H46F), C46(H46A,H46B,H46C), C34(H34A,H34B,
 H34C), C38(H38A,H38B,H38C)
;
_olex2_submission_special_instructions 'No special instructions were received'