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_7044066
_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 H9 Cl5 Cu3 N6, 2(C8 H15 N2)'
_chemical_formula_sum            'C25 H39 Cl5 Cu3 N10'
_chemical_formula_weight         847.53
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-23
_audit_creation_method
;
Olex2 1.2
(compiled Aug 10 2017 17:44:14 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-08-23 deposited with the CCDC.
2017-08-31 downloaded from the CCDC.
;
_cell_angle_alpha                93.015(2)
_cell_angle_beta                 108.718(2)
_cell_angle_gamma                108.591(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2091(10)
_cell_length_b                   13.1368(12)
_cell_length_c                   13.3517(11)
_cell_measurement_reflns_used    9505
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.95
_cell_volume                     1738.4(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 0.999
_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  0.0756
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            37960
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.392
_diffrn_reflns_theta_min         2.947
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'microfocus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.236
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3286
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014) was used for absorption correction. wR2(int) was 0.1575 before and 0.1013 after correction. The Ratio of minimum to maximum transmission is 0.4407. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_description       irregular
_exptl_crystal_F_000             862
_exptl_crystal_recrystallization_method 'Diethyl ether vapour diffusion'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         8688
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0664P)^2^+0.9515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1300
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7006
_reflns_number_total             8688
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02472j2.cif
_cod_data_source_block           Complex1
_cod_database_code               7044066
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.730
_shelx_estimated_absorpt_t_min   0.594
_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. Restrained distances
 C7B-C6BB \\sim C7B-C6BA \\sim C6BA-C5B \\sim C6BB-C5B
 with sigma of 0.02
3. Others
 Sof(Cl2B)=1-FVAR(1)
 Sof(Cl2A)=FVAR(1)
 Fixed Sof: Cl1A(0.88) Cl1B(0.12) H5BC(0.67) H5BD(0.67) H5BA(0.33) H5BB(0.33)
 C6BB(0.67) H6BA(0.67) H6BB(0.67) H7BD(0.67) H7BE(0.67) H7BF(0.67) H7BA(0.33)
 H7BB(0.33) H7BC(0.33) C6BA(0.33) H6BC(0.33) H6BD(0.33)
4.a Secondary CH2 refined with riding coordinates:
 C4A(H4AA,H4AB), C5A(H5AA,H5AB), C6A(H6AA,H6AB), C4B(H4BA,H4BB), C5B(H5BC,
 H5BD), C5B(H5BA,H5BB), C6BB(H6BA,H6BB), C6BA(H6BC,H6BD)
4.b Me refined with riding coordinates:
 C7A(H7AA,H7AB,H7AC), C8A(H8AA,H8AB,H8AC), C8B(H8BA,H8BB,H8BC)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C1A(H1A), C2A(H2A), C3A(H3A), C1B(H1B), C2B(H2B), C3B(H3B)
4.d Idealised Me refined as rotating group:
 C7B(H7BD,H7BE,H7BF), C7B(H7BA,H7BB,H7BC)
;
_shelx_res_checksum              44419
_olex2_exptl_crystal_mounting_method 'Glass fiber'
_olex2_submission_original_sample_id 'Complex 1'
_olex2_submission_special_instructions 'No special instructions were received'