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_7232132
_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         'Cl3 H9 Mn N2 O2'
_chemical_formula_sum            'Cl3 H9 Mn N2 O2'
_chemical_formula_weight         230.38
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-11-06 deposited with the CCDC.
2018-12-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.648(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.54110(10)
_cell_length_b                   13.9707(3)
_cell_length_c                   9.9630(3)
_cell_measurement_reflns_used    1718
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.6710
_cell_measurement_theta_min      5.4740
_cell_volume                     770.44(3)
_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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_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    -55.00 -29.00   1.00    1.00    --  -41.91 -57.00   0.00   26
  2  \w   -114.00 -17.00   1.00    1.00    --  -41.91 -38.00-120.00   97
  3  \w   -114.00 -88.00   1.00    1.00    --  -41.91 -57.00   0.00   26
  4  \w      7.00  46.00   1.00    1.00    --   41.91 -99.00 120.00   39
  5  \w     53.00  83.00   1.00    1.00    --   41.91 -99.00 120.00   30
  6  \w     49.00 121.00   1.00    3.41    --  105.91-125.00 -30.00   72
  7  \w     36.00  94.00   1.00    3.41    --  105.91 -61.00 -30.00   58
  8  \w     84.00 177.00   1.00    3.41    --  105.91  30.00  90.00   93
  9  \w    153.00 178.00   1.00    3.41    --  105.91 128.00 175.00   25
 10  \w    102.00 155.00   1.00    3.41    --  105.91 125.00  90.00   53
 11  \w    110.00 164.00   1.00    3.41    --  105.91 125.00 -30.00   54
 12  \w     88.00 123.00   1.00    3.41    --  105.91  45.00-120.00   35
;
_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      0.0851158000
_diffrn_orient_matrix_UB_12      -0.0834542000
_diffrn_orient_matrix_UB_13      0.0914266000
_diffrn_orient_matrix_UB_21      0.0795274000
_diffrn_orient_matrix_UB_22      0.0717978000
_diffrn_orient_matrix_UB_23      0.1107771000
_diffrn_orient_matrix_UB_31      -0.2529322000
_diffrn_orient_matrix_UB_32      -0.0055776000
_diffrn_orient_matrix_UB_33      0.0576554000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2816
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         72.820
_diffrn_reflns_theta_min         5.457
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    22.989
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.986
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         1486
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0270
_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^)+(0.0332P)^2^+0.0115P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0688
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1376
_reflns_number_total             1486
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01901k2.cif
_cod_data_source_block           18_pjs042_HydMnCl3
_cod_depositor_comments
'Adding full bibliography for 7232129--7232133.cif.'
_cod_database_code               7232132
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O2(H2A,H2B), O1(H1A,H1B)
2.b Secondary CH2 refined with riding coordinates:
 N1(H1C,H1D)
2.c Idealised Me refined as rotating group:
 N2(H2C,H2D,H2E)
;
_olex2_date_sample_data_collection 2018-01-18
_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 1.463
_oxdiff_exptl_absorpt_empirical_full_min 0.854