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_7048346
_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, C11 H24 N O'
_chemical_formula_sum            'C26 H27 F18 Mg N O7'
_chemical_formula_weight         831.79
_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                 91.129(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4523(8)
_cell_length_b                   18.8574(16)
_cell_length_c                   18.6567(16)
_cell_measurement_reflns_used    9805
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.219
_cell_measurement_theta_min      2.397
_cell_volume                     3324.8(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 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0382
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24991
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.405
_diffrn_reflns_theta_min         2.160
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6503
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1109 before and 0.0482 after correction. The Ratio of minimum to maximum transmission is 0.8727. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_description       plate
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.331
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         6109
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0530P)^2^+2.7868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1188
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4551
_reflns_number_total             6109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04364g2.cif
_cod_data_source_block           kcl-101disorder_pl
_cod_depositor_comments
'Adding full bibliography for 7048346--7048349.cif.'
_cod_database_code               7048346
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.937
_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
 C35-C34 = C36-C35 = C37-C36 = C34-C33
 1.5 with sigma of 0.05
 C35-C37
 2.6 with sigma of 0.05
3. Rigid body (RIGU) restrains
 C37, C36, C35, C34, C33, C32, C31, C30, C28, C27, N2, O8, N2, C29
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Fixed Sof: O7(0.757) N1(0.757) C21(0.757) H21A(0.757) H21B(0.757) C20(0.757)
 H20A(0.757) H20B(0.757) C26(0.757) H26A(0.757) H26B(0.757) H26C(0.757)
 C22(0.757) H22A(0.757) H22B(0.757) C18(0.757) H18A(0.757) H18B(0.757)
 C25(0.757) H25A(0.757) H25B(0.757) H25C(0.757) C16(0.757) H16A(0.757)
 H16B(0.757) C17(0.757) H17A(0.757) H17B(0.757) C19(0.757) H19A(0.757)
 H19B(0.757) C24(0.757) H24A(0.757) H24B(0.757) C23(0.757) H23A(0.757)
 H23B(0.757) O8(0.243) N2(0.243) C29(0.243) H29A(0.243) H29B(0.243) C27(0.243)
 H27A(0.243) H27B(0.243) C34(0.243) H34A(0.243) H34B(0.243) C28(0.243)
 H28A(0.243) H28B(0.243) C31(0.243) H31A(0.243) H31B(0.243) H31C(0.243)
 C30(0.243) H30A(0.243) H30B(0.243) C33(0.243) H33A(0.243) H33B(0.243)
 C32(0.243) H32A(0.243) H32B(0.243) C35(0.243) H35A(0.243) H35B(0.243)
 C36(0.243) H36A(0.243) H36B(0.243) C37(0.243) H37A(0.243) H37B(0.243)
 H37C(0.243)
5.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C20(H20A,H20B), C22(H22A,H22B), C18(H18A,H18B), C16(H16A,
 H16B), C17(H17A,H17B), C19(H19A,H19B), C24(H24A,H24B), C23(H23A,H23B),
 C29(H29A,H29B), C27(H27A,H27B), C34(H34A,H34B), C28(H28A,H28B), C30(H30A,H30B),
  C33(H33A,H33B), C32(H32A,H32B), C35(H35A,H35B), C36(H36A,H36B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C13(H13), C8(H8)
5.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C31(H31A,H31B,H31C), C37(H37A,H37B,
 H37C)
;
_olex2_submission_special_instructions 'No special instructions were received'