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_7232131
_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         'Cl5 H5 Mn N2, 2(H5 N2)'
_chemical_formula_sum            'Cl5 H15 Mn N6'
_chemical_formula_weight         331.37
_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     direct
_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                 94.423(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9779(4)
_cell_length_b                   10.9705(4)
_cell_length_c                   11.7726(5)
_cell_measurement_reflns_used    4466
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.2820
_cell_measurement_theta_min      4.3520
_cell_volume                     1156.05(8)
_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 0.998
_diffrn_measured_fraction_theta_max 0.869
_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    -14.00  29.00   1.00   10.00    --   11.79  57.00 -60.00   43
  2  \w     50.00  76.00   1.00   10.00    --   11.79  57.00 -60.00   26
  3  \w     50.00  83.00   1.00   10.00    --   11.79  57.00 -90.00   33
  4  \w     14.00  86.00   1.00   10.00    --   11.79  38.00-150.00   72
  5  \w      1.00  30.00   1.00   10.00    --  -10.46 -99.00-150.00   29
  6  \w    -20.00  46.00   1.00   10.00    --   11.79 -99.00  30.00   66
  7  \w    -20.00  46.00   1.00   10.00    --   11.79 -99.00 120.00   66
;
_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      0.0606679000
_diffrn_orient_matrix_UB_12      -0.0357274000
_diffrn_orient_matrix_UB_13      0.0234452000
_diffrn_orient_matrix_UB_21      0.0214167000
_diffrn_orient_matrix_UB_22      0.0479266000
_diffrn_orient_matrix_UB_23      0.0383027000
_diffrn_orient_matrix_UB_31      -0.0462451000
_diffrn_orient_matrix_UB_32      -0.0246059000
_diffrn_orient_matrix_UB_33      0.0404633000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.869
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10289
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.786
_diffrn_reflns_theta_min         3.321
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.262
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64560
_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_colour_primary    colourless
_exptl_crystal_density_diffrn    1.904
_exptl_crystal_description       block
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.246
_exptl_crystal_size_mid          0.221
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2878
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0309P)^2^+1.1186P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0801
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2432
_reflns_number_total             2878
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01901k2.cif
_cod_data_source_block           18_pjs_044_Hyd3MnCl5
_cod_depositor_comments
'Adding full bibliography for 7232129--7232133.cif.'
_cod_original_cell_volume        1156.05(9)
_cod_database_code               7232131
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.886
_shelx_estimated_absorpt_t_min   0.606
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups, All N(H,H,H) groups
2.a Rotating group:
 N5(H5A,H5B), N3(H3A,H3B)
2.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
2.c Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N6(H6A,H6B,H6C), N4(H4A,H4B,H4C)
;
_olex2_date_sample_data_collection 2018-01-25
_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 1.221
_oxdiff_exptl_absorpt_empirical_full_min 0.775