Low dimensional and frustrated antiferromagnetic interactions in transition metal chloride complexes with simple amine ligands
Chalmers, James E.; Srivastava, Anant Kumar; Dixey, Richard J. C.; Sivakumaran, Krrishna; Saines, Paul J.; CrystEngComm 21 (2019) 894–; doi:10.1039/C8CE01901K

data_7232133
_publ_section_title
;
 Low dimensional and frustrated antiferromagnetic interactions in
 transition metal chloride complexes with simple amine ligands
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              894
_journal_paper_doi               10.1039/C8CE01901K
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C2 H10 Cl2 Cu N2 O2'
_chemical_formula_sum            'C2 H10 Cl2 Cu N2 O2'
_chemical_formula_weight         228.56
_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     direct
_audit_creation_date             2018-07-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-06 deposited with the CCDC.
2018-12-27 downloaded from the CCDC.
;
_cell_angle_alpha                99.853(12)
_cell_angle_beta                 98.563(12)
_cell_angle_gamma                91.568(13)
_cell_formula_units_Z            1
_cell_length_a                   3.7868(6)
_cell_length_b                   5.6827(9)
_cell_length_c                   8.7079(11)
_cell_measurement_reflns_used    2099
_cell_measurement_temperature    150.0(4)
_cell_measurement_theta_max      75.8200
_cell_measurement_theta_min      5.1350
_cell_volume                     182.30(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      150.0(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2774
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -115.00 -17.00   1.00    4.00    --  -41.22 -38.00 -60.00   98
  2  \w   -115.00 -17.00   1.00    4.00    --  -41.22 -38.00  30.00   98
  3  \w    -35.00  74.00   1.00    4.00    --   41.22 -77.00-150.00  109
  4  \w     23.00  97.00   1.00    4.00    --   41.22-125.00-150.00   74
  5  \w     86.00 178.00   1.00    8.00    --  112.00  45.00 -90.00   92
  6  \w     29.00 109.00   1.00    8.00    --  112.00 -94.00  60.00   80
  7  \w     39.00 138.00   1.00    8.00    --  112.00 -45.00  30.00   99
  8  \w     36.00 116.00   1.00    8.00    --  112.00-111.00 -60.00   80
  9  \w    100.00 178.00   1.00    8.00    --  112.00 111.00 120.00   78
 10  \w     86.00 178.00   1.00    8.00    --  112.00  45.00-150.00   92
 11  \w    100.00 178.00   1.00    8.00    --  112.00 111.00  90.00   78
 12  \w     29.00 109.00   1.00    8.00    --  112.00 -94.00 -30.00   80
 13  \w     57.00 151.00   1.00    8.00    --  112.00 178.00 -90.00   94
 14  \w     57.00 151.00   1.00    8.00    --  112.00 178.00 -30.00   94
 15  \w     79.00 178.00   1.00    8.00    --  112.00  77.00   0.00   99
 16  \w   -113.00 -65.00   1.00    4.00    --  -41.22-138.00-112.00   48
 17  \w   -113.00 -13.00   1.00    4.00    --  -41.22 -57.00-120.00  100
 18  \w   -113.00 -13.00   1.00    4.00    --  -41.22 -57.00 150.00  100
 19  \w      9.00 117.00   1.00    4.00    --   41.22  77.00  30.00  108
 20  \w      1.00  82.00   1.00    4.00    --   41.22 -99.00 -60.00   81
 21  \w     83.00 178.00   1.00    8.00    --  112.00  61.00 150.00   95
 22  \w     79.00 178.00   1.00    8.00    --  112.00  77.00  30.00   99
 23  \w     84.00 178.00   1.00    8.00    --  112.00  30.00  90.00   94
 24  \w     79.00 178.00   1.00    8.00    --  112.00  77.00-150.00   99
 25  \w     84.00 178.00   1.00    8.00    --  112.00  30.00  60.00   94
 26  \w     84.00 178.00   1.00    8.00    --  112.00  30.00 -60.00   94
 27  \w     83.00 178.00   1.00    8.00    --  112.00  61.00-180.00   95
 28  \w     79.00 178.00   1.00    8.00    --  112.00  77.00 -30.00   99
 29  \w     86.00 178.00   1.00    8.00    --  112.00  45.00 150.00   92
 30  \w     83.00 178.00   1.00    8.00    --  112.00  61.00 -60.00   95
 31  \w     79.00 178.00   1.00    8.00    --  112.00  77.00  90.00   99
 32  \w     83.00 178.00   1.00    8.00    --  112.00  61.00-150.00   95
 33  \w     83.00 178.00   1.00    8.00    --  112.00  61.00   0.00   95
 34  \w     86.00 178.00   1.00    8.00    --  112.00  45.00  90.00   92
 35  \w     86.00 178.00   1.00    8.00    --  112.00  45.00 -30.00   92
 36  \w      1.00  82.00   1.00    4.00    --   41.22 -99.00  90.00   81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1419345000
_diffrn_orient_matrix_UB_12      0.2435673000
_diffrn_orient_matrix_UB_13      -0.0275258000
_diffrn_orient_matrix_UB_21      0.0975195000
_diffrn_orient_matrix_UB_22      0.0839496000
_diffrn_orient_matrix_UB_23      0.1796178000
_diffrn_orient_matrix_UB_31      0.3743037000
_diffrn_orient_matrix_UB_32      -0.0977781000
_diffrn_orient_matrix_UB_33      -0.0051546000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3563
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         76.510
_diffrn_reflns_theta_min         5.219
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.472
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.082
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             115
_exptl_crystal_size_max          0.163
_exptl_crystal_size_mid          0.022
_exptl_crystal_size_min          0.018
_refine_diff_density_max         1.151
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         759
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+0.0338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                715
_reflns_number_total             759
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01901k2.cif
_cod_data_source_block           18_pjs_019_MHA2CuCl2
_cod_depositor_comments
'Adding full bibliography for 7232129--7232133.cif.'
_cod_database_code               7232133
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Cu C O N H'
_shelx_estimated_absorpt_t_max   0.834
_shelx_estimated_absorpt_t_min   0.280
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
2.b Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E)
;
_olex2_date_sample_data_collection 2017-10-25
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.416
_oxdiff_exptl_absorpt_empirical_full_min 0.788