Towards ionic liquids with tailored magnetic properties: bmim+ salts of ferro- and antiferromagnetic CuII3 triangles
Boudalis, Athanassios; Rogez, Guillaume; Heinrich, Benoît; Raptis, Raphael; Turek, Philippe; Dalton Trans.  (2017) –; doi:10.1039/C7DT02472J

data_7044067
_publ_section_title
;
 Towards ionic liquids with tailored magnetic properties: bmim+ salts of
 ferro- and antiferromagnetic CuII3 triangles
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02472J
_journal_year                    2017
_chemical_formula_moiety         'C9 H10 Cl4 Cu3 N6 O, 2(C8 H15 N2)'
_chemical_formula_sum            'C25 H40 Cl4 Cu3 N10 O'
_chemical_formula_weight         829.09
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-08
_audit_creation_method
;
Olex2 1.2
(compiled Dec 12 2016 15:58:59 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-08-08 deposited with the CCDC.
2017-08-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5442(6)
_cell_length_b                   15.6305(9)
_cell_length_c                   19.9973(11)
_cell_measurement_reflns_used    9756
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.99
_cell_volume                     3608.3(3)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.15
_diffrn_detector                 'CMOS area detector'
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Bruker D8 QUEST CMOS'
_diffrn_measurement_device_type  'Bruker D8 QUEST CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1184
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            163883
_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         28.395
_diffrn_reflns_theta_min         2.994
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'microfocus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.083
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1669 before and 0.1224 after correction.
The Ratio of minimum to maximum transmission is 0.4568.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       prism
_exptl_crystal_F_000             1692
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.15(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         9003
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0440P)^2^+2.7767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1107
_reflns_Friedel_coverage         0.805
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                6736
_reflns_number_total             9003
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02472j2.cif
_cod_data_source_block           Complex3
_cod_database_code               7044067
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.85(2) 0.15(2)
2. 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 O(H) groups
3. Restrained distances
 C5AA-C4A = C5AB-C4A
 1.53 with sigma of 0.02
 C6AA-C5AA = C7AA-C6AA
 1.53 with sigma of 0.02
 C7AB-C6AB = C6AB-C5AB
 1.53 with sigma of 0.02
4. Rigid bond restraints
 C4A, C5AB, C6AB, C7AB, C4B, C5B, C6B, C7B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C4A \\sim C5AB \\sim C6AB \\sim C7AB \\sim C4B \\sim C5B \\sim C6B \\sim C7B:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C7AA) = Uanis(C7AB)
Uanis(C6AA) = Uanis(C6AB)
Uanis(C5AA) = Uanis(C5AB)
6. Rigid body (RIGU) restrains
 N1A, N2A, C1A, H1A, C2A, H2A, C3A, H3A, C4A, H4AC, H4AD, H4AA, H4AB, C5AB,
 H5AA, H5AB, C6AB, H6AA, H6AB, C7AB, H7AA, H7AB, H7AC, C8A, H8AA, H8AB, H8AC,
 C6AA, H6AC, H6AD, C7AA, H7AD, H7AE, H7AF, C5AA, H5AC, H5AD
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: H4AC(0.5) H4AD(0.5) H4AA(0.5) H4AB(0.5) C5AB(0.5) H5AA(0.5)
 H5AB(0.5) C6AB(0.5) H6AA(0.5) H6AB(0.5) C7AB(0.5) H7AA(0.5) H7AB(0.5)
 H7AC(0.5) C6AA(0.5) H6AC(0.5) H6AD(0.5) C7AA(0.5) H7AD(0.5) H7AE(0.5)
 H7AF(0.5) C5AA(0.5) H5AC(0.5) H5AD(0.5)
8.a Riding coordinates:
 O1(H1)
8.b Secondary CH2 refined with riding coordinates:
 C4A(H4AC,H4AD), C4A(H4AA,H4AB), C5AB(H5AA,H5AB), C6AB(H6AA,H6AB), C4B(H4BA,
 H4BB), C5B(H5BA,H5BB), C6B(H6BA,H6BB), C6AA(H6AC,H6AD), C5AA(H5AC,H5AD)
8.c Aromatic/amide H refined with riding coordinates:
 C1(H1B), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C1A(H1A), C2A(H2A), C3A(H3A), C1B(H1BA), C2B(H2B), C3B(H3B)
8.d Idealised Me refined as rotating group:
 C7AB(H7AA,H7AB,H7AC), C8A(H8AA,H8AB,H8AC), C7B(H7BA,H7BB,H7BC), C8B(H8BA,H8BB,
 H8BC), C7AA(H7AD,H7AE,H7AF)
;
_shelx_res_checksum              2995
_olex2_exptl_crystal_mounting_method 'glass fibre'
_olex2_submission_original_sample_id AKB16
_olex2_submission_special_instructions 'No special instructions were received'