A simple methodology for constructing ferromagnetically coupled Cr(iii) compounds.
Fraser, Hector W. L.; Smythe, Lucy; Dey, Sourav; Nichol, Gary S.; Piligkos, Stergios; Rajaraman, Gopalan; Brechin, Euan K.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 8100–8109; doi:10.1039/c8dt01963k

data_7046487
_publ_section_title
;
 A simple methodology for constructing ferromagnetically coupled Cr(iii)
 compounds.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8100
_journal_page_last               8109
_journal_paper_doi               10.1039/c8dt01963k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C17 H29 Cl2 Cr2 N2 O6, Cl'
_chemical_formula_sum            'C17 H29 Cl3 Cr2 N2 O6'
_chemical_formula_weight         567.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-25
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2017-10-12 deposited with the CCDC.
2018-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.560(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1908(3)
_cell_length_b                   10.41623(19)
_cell_length_c                   14.1087(3)
_cell_measurement_reflns_used    22700
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      31.0080
_cell_measurement_theta_min      3.9730
_cell_volume                     2331.13(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43h (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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.937
_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    -20.00  27.00   1.00    4.00    --  -13.24 -99.00 -60.00   47
  2  \w    -20.00  27.00   1.00    4.00    --  -13.24 -99.00 120.00   47
  3  \w     -8.00  87.00   1.00    4.00    --   14.65  38.00 -90.00   95
  4  \w     35.00 101.00   1.00    4.00    --   14.65 178.00-150.00   66
  5  \w    -58.00  37.00   1.00    4.00    --   14.65 -38.00 150.00   95
  6  \w     35.00 101.00   1.00    4.00    --   14.65 178.00 150.00   66
  7  \w    -20.00  55.00   1.00    4.00    --   14.65 -99.00 150.00   75
  8  \w     -8.00  87.00   1.00    4.00    --   14.65  38.00   0.00   95
  9  \w    -40.00  57.00   1.00    4.00    --  -13.24  57.00 -60.00   97
 10  \w     -8.00  19.00   1.00    4.00    --   14.65  38.00 120.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0442823000
_diffrn_orient_matrix_UB_12      0.0094161000
_diffrn_orient_matrix_UB_13      0.0113576000
_diffrn_orient_matrix_UB_21      0.0047942000
_diffrn_orient_matrix_UB_22      -0.0576691000
_diffrn_orient_matrix_UB_23      0.0273035000
_diffrn_orient_matrix_UB_31      0.0041044000
_diffrn_orient_matrix_UB_32      -0.0349292000
_diffrn_orient_matrix_UB_33      -0.0419367000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48698
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.306
_diffrn_reflns_theta_min         2.970
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.311
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.351
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43h (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_recrystallization_method
'The material was recrystallised from acetonitrile by hydrothermal bomb'
_exptl_crystal_size_max          0.471
_exptl_crystal_size_mid          0.282
_exptl_crystal_size_min          0.194
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         7156
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0286
_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^)+(0.0281P)^2^+1.5432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0696
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6488
_reflns_number_total             7156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01963k2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7046484--7046487.cif.'
_cod_original_cell_volume        2331.11(8)
_cod_database_code               7046487
_chemical_oxdiff_formula         'C30 H30 N10 O10 Cr Cl Na'
_chemical_oxdiff_usercomment     '@ 120 K L145'
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              22966
_shelx_shelxl_version_number     2016/6
_olex2_date_sample_data_collection 2016-11-24
_olex2_date_sample_submission    2016-11-24
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id L145
_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 1.354
_oxdiff_exptl_absorpt_empirical_full_min 0.806