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_7043484
_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_absolute_configuration ad
_chemical_formula_moiety         'C24 H16 Cl6 Cr2 N6, 3(C5 H9 N O)'
_chemical_formula_sum            'C39 H43 Cl6 Cr2 N9 O3'
_chemical_formula_weight         1002.52
_space_group_crystal_system      trigonal
_space_group_IT_number           145
_space_group_name_Hall           'P 32'
_space_group_name_H-M_alt        'P 32'
_symmetry_space_group_name_Hall  'P 32'
_symmetry_space_group_name_H-M   'P 32'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-01-20
_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                120
_cell_formula_units_Z            6
_cell_length_a                   18.90091(13)
_cell_length_b                   18.90091(13)
_cell_length_c                   21.1210(2)
_cell_measurement_reflns_used    26009
_cell_measurement_temperature    180.1(3)
_cell_measurement_theta_max      73.3500
_cell_measurement_theta_min      4.6440
_cell_volume                     6534.47(9)
_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      180.1(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 0.997
_diffrn_measurement_details
;
  1 omega  -47.00   29.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.9365   38.0000  -90.0000 76

  2 omega    7.00   77.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       38.9365  -99.0000 -180.0000 70

  3 omega   29.00   82.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -30.0000 -120.0000 53

  4 omega   37.00  108.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -94.0000    0.0000 71

  5 omega   96.00  140.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -61.0000   30.0000 44

  6 omega   47.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -30.0000  150.0000 44

  7 omega   46.00   74.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -61.0000   30.0000 28

  8 omega  100.00  141.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  111.0000  -90.0000 41

  9 omega  -77.00   -8.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.0615  -38.0000   60.0000 69

 10 omega  -37.00   -3.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.0615  -77.0000    0.0000 34

 11 omega  -80.00   -9.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.0615  -57.0000   30.0000 71

 12 omega -113.00  -80.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.0615  -99.0000   30.0000 33

 13 omega   77.00  102.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000   30.0000 25

 14 omega   77.00  103.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000  120.0000 26

 15 omega   77.00  103.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000   90.0000 26

 16 omega   74.00  100.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000   60.0000 26

 17 omega   77.00  103.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000   60.0000 26

 18 omega   74.00  100.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000   90.0000 26

 19 omega   75.00  101.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000  120.0000 26

 20 omega   79.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   45.0000  120.0000 42

 21 omega  129.00  158.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   45.0000  120.0000 29

 22 omega   79.00  105.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   45.0000   60.0000 26

 23 omega   81.00  107.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   45.0000   90.0000 26

 24 omega   74.00  100.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000   30.0000 26

 25 omega  109.00  134.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000   90.0000 25

 26 omega   77.00  112.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   30.0000  120.0000 35

 27 omega  153.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   30.0000   60.0000 25

 28 omega   76.00  102.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000    0.0000 26

 29 omega   82.00  127.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   30.0000   90.0000 45

 30 omega   72.00  134.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   30.0000   60.0000 62

 31 omega  -41.00   35.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.0615   38.0000   30.0000 76

 32 omega  -43.00  -17.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.0615  125.0000  120.0000 26

 33 omega -119.00  -87.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.0615  -99.0000  150.0000 32

 34 omega   20.00   72.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       39.0615  -99.0000  -60.0000 52

 35 omega   58.00   84.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   15.0000 -180.0000 26

 36 omega   40.00   77.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -30.0000  120.0000 37

 37 omega  100.00  126.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  178.0000  -90.0000 26

 38 omega   56.00   87.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -45.0000 -120.0000 31

 39 omega   52.00   78.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -30.0000  -90.0000 26

 40 omega   54.00   79.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -30.0000 -180.0000 25

 41 omega   54.00  116.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499 -111.0000  120.0000 62

 42 omega   51.00  107.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -94.0000  -90.0000 56

 43 omega  116.00  171.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   15.0000 -180.0000 55

 44 omega   23.00  108.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -94.0000 -150.0000 85
;
_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      -0.0459466000
_diffrn_orient_matrix_UB_12      -0.0940221000
_diffrn_orient_matrix_UB_13      -0.0033391000
_diffrn_orient_matrix_UB_21      -0.0805868000
_diffrn_orient_matrix_UB_22      -0.0004738000
_diffrn_orient_matrix_UB_23      -0.0122217000
_diffrn_orient_matrix_UB_31      0.0158387000
_diffrn_orient_matrix_UB_32      0.0044679000
_diffrn_orient_matrix_UB_33      -0.0718279000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0790
_diffrn_reflns_av_unetI/netI     0.0649
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            63252
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.680
_diffrn_reflns_theta_max         73.421
_diffrn_reflns_theta_min         3.416
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.901
_exptl_absorpt_correction_T_max  0.819
_exptl_absorpt_correction_T_min  0.289
_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    1.529
_exptl_crystal_description       plate
_exptl_crystal_F_000             3084
_exptl_crystal_size_max          0.2869
_exptl_crystal_size_mid          0.0997
_exptl_crystal_size_min          0.027
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1072
_refine_ls_number_reflns         16355
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0684P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1140
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                15489
_reflns_number_total             16355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01747b2.cif
_cod_data_source_block           compound11
_cod_original_cell_volume        6534.46(12)
_cod_database_code               7043484
_chemical_oxdiff_formula         'C39 H43 Cl6 Cr2 N9 O3'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.546(9) 0.450(5) 0.003(5) 0.001(5)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C85(H85A,H85B), C86(H86A,H86B), C84(H84A,H84B), C65(H65A,H65B), C64(H64A,
 H64B), C63(H63A,H63B), C78(H78A,H78B), C79(H79A,H79B), C77(H77A,H77B),
 C93(H93A,H93B), C91(H91A,H91B), C92(H92A,H92B), C70(H70A,H70B), C71(H71A,H71B),
  C72(H72A,H72B), C100(H10D,H10E), C98(H98A,H98B), C99(H99A,H99B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C10(H10), C28(H28), C18(H18), C15(H15), C8(H8), C19(H19), C22(H22),
 C30(H30), C27(H27), C16(H16), C9(H9), C29(H29), C21(H21), C17(H17), C20(H20),
 C59(H59), C52(H52), C60(H60), C38(H38), C46(H46), C47(H47), C57(H57), C50(H50),
  C37(H37), C51(H51), C49(H49), C45(H45), C39(H39), C48(H48), C40(H40), C58(H58)
3.c Idealised Me refined as rotating group:
 C88(H88A,H88B,H88C), C67(H67A,H67B,H67C), C81(H81A,H81B,H81C), C95(H95A,H95B,
 H95C), C74(H74A,H74B,H74C), C102(H10A,H10B,H10C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'