CrIII as an alternative to RuII in metallo-supramolecular chemistry
Zare, Davood; Doistau, Benjamin; Nozary, Homayoun; Besnard, Céline; Guénée, Laure; Suffren, Yan; Pelé, Anne-Laure; Hauser, Andreas; Piguet, Claude; Dalton Trans.  (2017) –; doi:10.1039/C7DT01747B

data_7043481
_publ_section_title
;
 CrIII as an alternative to RuII in metallo-supramolecular chemistry
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01747B
_journal_year                    2017
_chemical_formula_moiety         'C30 H20 Cl6 Cr2 N6'
_chemical_formula_sum            'C30 H20 Cl6 Cr2 N6'
_chemical_formula_weight         781.22
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-02-08
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.11.10 svn.r3248 for OlexSys, GUI svn.r5133)
;
_audit_update_record
;
2017-05-26 deposited with the CCDC.
2017-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.61144(9)
_cell_length_b                   13.61144(9)
_cell_length_c                   24.0699(3)
_cell_measurement_reflns_used    22489
_cell_measurement_temperature    179.9(3)
_cell_measurement_theta_max      73.2230
_cell_measurement_theta_min      4.5560
_cell_volume                     4459.46(7)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4679
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   34.00   60.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       38.9365 -130.0000  164.0000 26

  2 omega   80.00  170.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   45.0000   30.0000 90

  3 omega  140.00  176.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  111.0000 -120.0000 36

  4 omega  127.00  153.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  111.0000 -150.0000 26

  5 omega   43.00  116.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499 -111.0000 -120.0000 73

  6 omega -105.00  -67.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.9365 -140.0000   -8.0000 38

  7 omega -118.00  -79.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.9365  -99.0000  120.0000 39

  8 omega -122.00  -82.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.9365  -99.0000   60.0000 40

  9 omega -116.00  -69.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.9365  -57.0000   60.0000 47

 10 omega  -36.00   -2.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.9365   77.0000 -120.0000 34

 11 omega  -62.00  -13.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.9365  -38.0000   90.0000 49

 12 omega  -44.00  -19.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.9365  -57.0000   60.0000 25

 13 omega   81.00  106.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   45.0000  150.0000 25

 14 omega   43.00   72.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -94.0000  -90.0000 29

 15 omega  153.00  178.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000   90.0000 25

 16 omega  111.00  141.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  111.0000  -30.0000 30

 17 omega   77.00  103.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000   90.0000 26

 18 omega   79.00  105.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   45.0000  120.0000 26

 19 omega   84.00  121.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   30.0000  150.0000 37

 20 omega   74.00  100.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000  120.0000 26

 21 omega  145.00  175.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000  120.0000 30

 22 omega   74.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   30.0000  120.0000 41

 23 omega   77.00  102.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000  120.0000 25

 24 omega   74.00  100.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000   90.0000 26

 25 omega -121.00  -86.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.9365  -99.0000 -180.0000 35

 26 omega  -86.00  -52.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.9365   19.0000  120.0000 34

 27 omega    2.00   36.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.9365   19.0000  120.0000 34

 28 omega  -27.00   -1.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.9365   19.0000  120.0000 26

 29 omega   12.00   71.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       38.9365  -99.0000   60.0000 59

 30 omega    4.00   69.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       38.9365  -99.0000  -30.0000 65

 31 omega   69.00  127.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       38.9365  178.0000  -60.0000 58

 32 omega  115.00  147.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  178.0000 -120.0000 32

 33 omega   75.00  101.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  178.0000 -120.0000 26

 34 omega   30.00  141.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -77.0000  -60.0000 111

 35 omega   74.00  109.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499 -111.0000   90.0000 35

 36 omega   68.00  116.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499 -111.0000  -60.0000 48

 37 omega   33.00  101.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -94.0000 -180.0000 68

 38 omega   32.00   58.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499 -111.0000   90.0000 26

 39 omega   29.00  147.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -30.0000 -180.0000 118

 40 omega  102.00  154.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   15.0000 -180.0000 52

 41 omega   43.00   81.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   15.0000 -180.0000 38
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1062101000
_diffrn_orient_matrix_UB_12      -0.0322474000
_diffrn_orient_matrix_UB_13      0.0126514000
_diffrn_orient_matrix_UB_21      -0.0390653000
_diffrn_orient_matrix_UB_22      0.0929417000
_diffrn_orient_matrix_UB_23      -0.0290584000
_diffrn_orient_matrix_UB_31      -0.0037808000
_diffrn_orient_matrix_UB_32      -0.0558972000
_diffrn_orient_matrix_UB_33      -0.0555962000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            40446
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.680
_diffrn_reflns_theta_max         73.352
_diffrn_reflns_theta_min         3.731
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.516
_exptl_absorpt_correction_T_max  0.505
_exptl_absorpt_correction_T_min  0.255
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) 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) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.2849
_exptl_crystal_size_mid          0.2198
_exptl_crystal_size_min          0.1444
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.

;
_refine_ls_abs_structure_Flack   0.013(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         4468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0495P)^2^+1.5267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0917
_reflns_Friedel_coverage         0.712
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                4242
_reflns_number_total             4468
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01747b2.cif
_cod_data_source_block           compound12
_cod_database_code               7043481
_chemical_oxdiff_formula         'C30 H20 Cl6 Cr2 N6'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.987(8) 0.013(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C17(H17), C18(H18), C7(H7), C6(H6), C5(H5), C16(H16), C0AA(H0AA),
 C12(H12), C10(H10)
;
_shelx_fab_checksum              39413
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'