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_7043476
_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
'C60 H42 Cr2 N12, 6(F6 P), 8(C2 H3 N), C4 H10 O'
_chemical_formula_sum            'C80 H76 Cr2 F36 N20 O P6'
_chemical_formula_weight         2307.42
_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   geom
_audit_creation_date             2015-10-06
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-04-05 deposited with the CCDC.
2017-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                65.495(2)
_cell_angle_beta                 82.9117(19)
_cell_angle_gamma                81.9267(19)
_cell_formula_units_Z            2
_cell_length_a                   11.6319(3)
_cell_length_b                   20.7157(5)
_cell_length_c                   22.6001(5)
_cell_measurement_reflns_used    32946
_cell_measurement_temperature    180(1)
_cell_measurement_theta_max      73.4770
_cell_measurement_theta_min      3.7760
_cell_volume                     4893.3(2)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4679
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details
;
  1 omega  -47.00   28.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.9365   38.0000 -120.0000 75

  2 omega   -3.00   22.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0000   94.0000   40.0307 25

  3 omega   19.00   44.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   81.0000   37.8585 25

  4 omega   32.00   58.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   77.0000   52.7791 26

  5 omega   32.00   63.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   77.0000   83.1463 31

  6 omega   89.00  149.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   77.0000   83.1463 60

  7 omega  108.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000    0.0000 70

  8 omega  151.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000  -90.0000 27

  9 omega  150.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000  -90.0000 28

 10 omega  120.00  152.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000 -150.0000 32

 11 omega  107.00  145.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   77.0000 -179.7664 38

 12 omega  108.00  176.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000 -180.0000 68

 13 omega  107.00  149.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000  -30.0000 42

 14 omega  111.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000   30.0000 67

 15 omega   99.00  149.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   77.0000  136.9580 50

 16 omega   77.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000  120.0000 26

 17 omega   78.00  110.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000   90.0000 32

 18 omega   77.00  107.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000   60.0000 30

 19 omega   74.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000  120.0000 104

 20 omega   94.00  156.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000   77.0000  -82.5596 62

 21 omega   77.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000  -90.0000 26

 22 omega   75.00  141.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000  -90.0000 66

 23 omega   78.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000 -150.0000 25

 24 omega   77.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000 -180.0000 26

 25 omega   74.00  175.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000 -120.0000 101

 26 omega   78.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000   30.0000 25

 27 omega   74.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000    0.0000 25

 28 omega   74.00  100.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000   30.0000 26

 29 omega   74.00  146.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000   60.0000 72

 30 omega   74.00  154.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000  150.0000 80

 31 omega   74.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000   90.0000 104

 32 omega   77.00  140.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000 -120.0000 63

 33 omega   74.00  100.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000 -180.0000 26

 34 omega   74.00  100.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000 -150.0000 26

 35 omega   64.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   76.0000  -48.6213 114

 36 omega   74.00  100.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000  -30.0000 26

 37 omega   42.00   85.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       76.0000   71.0000    3.2122 43

 38 omega   32.00   59.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   75.0000  -32.3835 27

 39 omega   36.00   72.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000   77.0000  -82.5596 36

 40 omega   32.00   75.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   77.0000 -152.7380 43

 41 omega   45.00   82.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       76.0000   56.0000 -177.3985 37

 42 omega   28.00   54.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       64.0000   77.0000 -100.0919 26

 43 omega   20.00   46.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   81.0000  -36.5115 26

 44 omega   19.00   44.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   81.0000    7.4608 25

 45 omega   16.00   43.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       52.0000   81.0000  -82.1038 27

 46 omega    3.00   28.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0000   90.0000 -125.7316 25

 47 omega   32.00   57.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   77.0000 -179.7664 25

 48 omega   36.00  101.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -94.0000   30.0000 65

 49 omega   49.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -94.0000  150.0000 44

 50 omega   24.00  108.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -94.0000   90.0000 84

 51 omega   28.00  108.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -94.0000  -60.0000 80

 52 omega   55.00  129.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       38.9365 -178.0000 -180.0000 74

 53 omega   37.00   89.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499 -111.0000 -120.0000 52
;
_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      0.1033602000
_diffrn_orient_matrix_UB_12      0.0213702000
_diffrn_orient_matrix_UB_13      0.0221346000
_diffrn_orient_matrix_UB_21      0.0854674000
_diffrn_orient_matrix_UB_22      -0.0387925000
_diffrn_orient_matrix_UB_23      -0.0351032000
_diffrn_orient_matrix_UB_31      0.0002577000
_diffrn_orient_matrix_UB_32      0.0691662000
_diffrn_orient_matrix_UB_33      -0.0626056000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            69658
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.426
_diffrn_reflns_theta_min         3.782
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.875
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_correction_T_min  0.265
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_description       plate
_exptl_crystal_F_000             2332
_exptl_crystal_size_max          0.8178
_exptl_crystal_size_mid          0.2444
_exptl_crystal_size_min          0.0329
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1371
_refine_ls_number_reflns         18913
_refine_ls_number_restraints     468
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0575
_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^)+(0.0972P)^2^+3.2131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1547
_refine_ls_wR_factor_ref         0.1636
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16085
_reflns_number_total             18913
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01747b2.cif
_cod_data_source_block           13
_cod_database_code               7043476
_chemical_oxdiff_formula         'C40 H38 Cr1 F18 N10 O0.5 P3'
_reflns_odcompleteness_completeness 97.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Restrained distances
 F3B-F2B \\sim F3B-F5B \\sim F3B-F1B \\sim F3B-F4B \\sim F2B-F1B \\sim F2B-F4B
\\sim F2B-F6B \\sim F6A-F4A
 \\sim F6A-F5A \\sim F6A-F2A \\sim F6A-F1A \\sim F5B-F1B \\sim F5B-F4B \\sim
F5B-F6B \\sim F4A-F3A \\sim F4A-
 F5A \\sim F4A-F2A \\sim F3A-F5A \\sim F3A-F2A \\sim F3A-F1A \\sim F1B-F6B
\\sim F5A-F1A \\sim F2A-F1A ~
 F4B-F6B
 with sigma of 0.04
 P1-F3B \\sim P1-F2B \\sim P1-F6A \\sim P1-F5B \\sim P1-F4A \\sim P1-F3A \\sim
P1-F1B \\sim P1-F5A \\sim P1-
 F2A \\sim P1-F4B \\sim P1-F1A \\sim P1-F6B
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 F1A, P1, F6A, F5B, F3A, F2A, F4B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1B, P1, F3B, F2B, F4A, F5A, F6B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F4B)=Sof(F5B)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F6A)=1-FVAR(1)
 Sof(F1B)=Sof(F3B)=Sof(F2B)=Sof(F6B)=Sof(F4A)=Sof(F5A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C153(H15D,H15E), C151(H15F,H15G)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C24(H24), C7(H7), C47(H47), C4(H4), C18(H18), C58(H58), C52(H52),
 C15(H15), C46(H46), C35(H35), C64(H64), C11(H11), C45(H45), C50(H50), C55(H55),
  C12(H12), C6(H6), C10(H10), C44(H44), C78(H78), C30(H30), C67(H67), C56(H56),
 C26(H26), C27(H27), C17(H17), C36(H36), C25(H25), C57(H57), C71(H71), C76(H76),
  C32(H32), C66(H66), C72(H72), C37(H37), C75(H75), C77(H77), C38(H38),
 C16(H16), C70(H70), C65(H65)
5.c Idealised Me refined as rotating group:
 C146(H14D,H14E,H14F), C2AA(H2AA,H2AB,H2AC), C154(H15A,H15B,H15C), C137(H13G,
 H13H,H13I), C149(H14A,H14B,H14C), C143(H14G,H14H,H14I), C140(H14J,H14K,H14L),
 C152(H15H,H15I,H15J), C134(H13D,H13E,H13F), C131(H13A,H13B,H13C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'