Voltage clustering in redox-active ligand complexes: mitigating electronic communication through choice of metal ion.
Zarkesh, Ryan A.; Ichimura, Andrew S.; Monson, Todd C.; Tomson, Neil C.; Anstey, Mitchell R.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 9962–9969; doi:10.1039/c6dt00422a

data_7038839
_publ_section_title
;
 Voltage clustering in redox-active ligand complexes: mitigating
 electronic communication through choice of metal ion.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9962
_journal_page_last               9969
_journal_paper_doi               10.1039/c6dt00422a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C84 H72 Cr1 N6'
_chemical_formula_sum            'C84 H72 Cr N6'
_chemical_formula_weight         1217.47
_chemical_melting_point          ?
_chemical_name_common            tri(dmp-BIAN)Cr
_chemical_name_systematic
'tri(N,N'-bis(3,5-dimethylphenylimino)acenaphthenesemiquinone) chromium'
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-12-11
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_audit_update_record
;
2016-01-19 deposited with the CCDC.
2016-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   13.1548(2)
_cell_length_b                   13.1548(2)
_cell_length_c                   71.8546(12)
_cell_measurement_reflns_used    17297
_cell_measurement_temperature    150.05(10)
_cell_measurement_theta_max      28.6770
_cell_measurement_theta_min      2.8860
_cell_volume                     10768.5(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.05(10)
_diffrn_detector_area_resol_mean 10.2358
_diffrn_measured_fraction_theta_full 0.897
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0248840000
_diffrn_orient_matrix_UB_12      0.0528495000
_diffrn_orient_matrix_UB_13      0.0052121000
_diffrn_orient_matrix_UB_21      -0.0556185000
_diffrn_orient_matrix_UB_22      -0.0175844000
_diffrn_orient_matrix_UB_23      0.0040203000
_diffrn_orient_matrix_UB_31      0.0127652000
_diffrn_orient_matrix_UB_32      -0.0278135000
_diffrn_orient_matrix_UB_33      0.0073595000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0097
_diffrn_reflns_Laue_measured_fraction_full 0.897
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       85
_diffrn_reflns_limit_l_min       -85
_diffrn_reflns_number            54503
_diffrn_reflns_point_group_measured_fraction_full 0.897
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.888
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.207
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.960
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             3852
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Slow evaporation of THF'
_exptl_crystal_size_max          0.2731
_exptl_crystal_size_mid          0.1665
_exptl_crystal_size_min          0.1041
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2119
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0764P)^2^+17.4878P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1279
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1963
_reflns_number_total             2119
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00422a2.cif
_cod_data_source_block           raz-01-078
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'n/a' was changed to '?' - the value
is undefined or not given.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7038837--7038842.cif.
;
_cod_original_cell_volume        10768.4(4)
_cod_database_code               7038839
_shelxl_version_number           2014-3
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C11(H11), C13(H13)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)

All atoms are refined anisotropically and protons are generated 
in calculated positions and refined using the riding model. A 
446.6 Ang^3 solvent accessible void is present in the unit cell (~4.1%)
that corresponds to a total of 126 electrons. Attempts to model the disordered
THF molecules resulted in an unstable refinement of the model. The solvent mask
routine in OLEX 2 was used to remove this void for the final refinement.

;
_shelx_res_checksum              83945