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_7232130
_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         'Cl6 Mn, 2(Cl4 H7 Mn N2 O), 2(Cl), 8(H5 N2)'
_chemical_formula_sum            'Cl16 H54 Mn3 N20 O2'
_chemical_formula_weight         1098.65
_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   mixed
_audit_creation_date             2018-11-01
_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                89.821(4)
_cell_angle_beta                 84.447(3)
_cell_angle_gamma                75.697(4)
_cell_formula_units_Z            1
_cell_length_a                   7.5839(3)
_cell_length_b                   9.1752(4)
_cell_length_c                   15.0656(6)
_cell_measurement_reflns_used    4133
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.8570
_cell_measurement_theta_min      4.9510
_cell_volume                     1010.82(7)
_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)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.965
_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    -26.00  35.00   1.00    1.00    --   41.91 -38.00 150.00   61
  2  \w      3.00  53.00   1.00    1.00    --   41.91 -99.00 120.00   50
  3  \w     40.00  87.00   1.00    1.06    --  105.91 -94.00  30.00   47
  4  \w     45.00 116.00   1.00    1.06    --  105.91-125.00 -60.00   71
  5  \w     57.00  96.00   1.00    1.00    --   41.91-125.00-150.00   39
  6  \w     53.00 124.00   1.00    1.06    --  105.91 -45.00-120.00   71
  7  \w     81.00 178.00   1.00    1.06    --  105.91  45.00 -60.00   97
  8  \w    150.00 176.00   1.00    1.06    --  105.91 125.00  90.00   26
  9  \w    106.00 142.00   1.00    1.06    --  105.91 125.00-120.00   36
 10  \w     35.00 142.00   1.00    1.06    --  105.91 -15.00 -60.00  107
 11  \w     44.00 114.00   1.00    1.06    --  105.91-125.00 120.00   70
 12  \w     42.00 131.00   1.00    1.06    --  105.91 -30.00 120.00   89
 13  \w     37.00 121.00   1.00    1.06    --  105.91 -77.00 120.00   84
 14  \w   -111.00 -10.00   1.00    1.00    --  -41.91 -77.00   0.00  101
 15  \w   -113.00 -25.00   1.00    1.00    --  -41.91 -38.00-120.00   88
;
_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      -0.0397005000
_diffrn_orient_matrix_UB_12      -0.1434958000
_diffrn_orient_matrix_UB_13      0.0417246000
_diffrn_orient_matrix_UB_21      -0.0829945000
_diffrn_orient_matrix_UB_22      0.0891190000
_diffrn_orient_matrix_UB_23      0.0869433000
_diffrn_orient_matrix_UB_31      -0.1895199000
_diffrn_orient_matrix_UB_32      0.0387957000
_diffrn_orient_matrix_UB_33      -0.0354980000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6591
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        68.000
_diffrn_reflns_theta_max         72.958
_diffrn_reflns_theta_min         4.975
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.584
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34674
_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    1.805
_exptl_crystal_description       block
_exptl_crystal_F_000             557
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3911
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0377P)^2^+0.4995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0818
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3644
_reflns_number_total             3911
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01901k2.cif
_cod_data_source_block           18_pjs041_Hyd10MnCl16
_cod_depositor_comments
'Adding full bibliography for 7232129--7232133.cif.'
_cod_original_cell_volume        1010.83(7)
_cod_database_code               7232130
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Cl Mn N O'
_reflns_odcompleteness_completeness 99.78
_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. Restrained distances
 N3-H3A = N3-H3B = N7-H7A = N7-H7B = N10-H10A = N10-H10B
 0.89 with sigma of 0.001
 H3A-H3B = H7A-H7B = H10A-H10B
 1.428 with sigma of 0.002
3.a Rotating group:
 O1(H1A,H1B), N5(H5A,H5B)
3.b Secondary CH2 refined with riding coordinates:
 N1(H1C,H1D)
3.c Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N9(H9A,H9B,H9C), N8(H8A,H8B,H8C), N4(H4A,H4B,H4C), N6(H6A,
 H6B,H6C)
;
_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 1.921
_oxdiff_exptl_absorpt_empirical_full_min 0.682