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_7043474
_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         'C62 H42 Cr2 N12, 6(F6 P), 10(C2 H3 N)'
_chemical_formula_sum            'C82 H72 Cr2 F36 N22 P6'
_chemical_formula_weight         2339.43
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-22
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-04-05 deposited with the CCDC.
2017-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                104.2876(14)
_cell_angle_beta                 90.8897(12)
_cell_angle_gamma                104.2657(14)
_cell_formula_units_Z            1
_cell_length_a                   10.18638(16)
_cell_length_b                   12.5709(2)
_cell_length_c                   21.0644(3)
_cell_measurement_reflns_used    18649
_cell_measurement_temperature    180.00(14)
_cell_measurement_theta_max      73.4740
_cell_measurement_theta_min      3.7210
_cell_volume                     2524.92(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4679
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_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     15.00  41.00   1.00    3.00    --   52.00  80.00 -94.64   26
  2  \w     32.00  58.00   1.00    3.00    --   68.00  76.00 -66.74   26
  3  \w     36.00  88.00   1.00    3.00    --   72.00  77.00 -37.99   52
  4  \w    103.00 145.00   1.00    3.00    --   68.00  76.00 -66.74   42
  5  \w    100.00 169.00   1.00    7.00    --  110.40 111.00 -60.00   69
  6  \w    116.00 143.00   1.00    7.00    --  110.40  61.00  30.00   27
  7  \w    113.00 144.00   1.00    7.00    --  110.40  77.00  60.00   31
  8  \w    100.00 177.00   1.00    7.00    --  110.40 111.00 -30.00   77
  9  \w    108.00 178.00   1.00    7.00    --  110.40  77.00-150.00   70
 10  \w    113.00 149.00   1.00    7.00    --  110.40  77.00-180.00   36
 11  \w     95.00 151.00   1.00    3.00    --   68.00  75.00-116.42   56
 12  \w     78.00 125.00   1.00    3.00    --   72.00  77.00-177.68   47
 13  \w     78.00 105.00   1.00    7.00    --  110.40  61.00-120.00   27
 14  \w     77.00 109.00   1.00    7.00    --  110.40  61.00-150.00   32
 15  \w     74.00 106.00   1.00    7.00    --  110.40  77.00-180.00   32
 16  \w     74.00 147.00   1.00    7.00    --  110.40  77.00-120.00   73
 17  \w     74.00 132.00   1.00    7.00    --  110.40  77.00 -60.00   58
 18  \w     79.00 108.00   1.00    7.00    --  110.40  61.00   0.00   29
 19  \w     77.00 105.00   1.00    7.00    --  110.40  61.00  60.00   28
 20  \w     77.00 106.00   1.00    7.00    --  110.40  61.00  30.00   29
 21  \w     74.00 177.00   1.00    7.00    --  110.40  77.00  90.00  103
 22  \w     94.00 143.00   1.00    3.00    --   60.00  75.00 131.74   49
 23  \w     77.00 103.00   1.00    7.00    --  110.40  61.00 120.00   26
 24  \w     78.00 110.00   1.00    7.00    --  110.40  61.00  90.00   32
 25  \w     74.00 148.00   1.00    7.00    --  110.40  77.00 120.00   74
 26  \w     74.00 177.00   1.00    7.00    --  110.40  77.00 150.00  103
 27  \w     74.00 114.00   1.00    7.00    --  110.40  77.00   0.00   40
 28  \w     74.00 100.00   1.00    7.00    --  110.40  77.00 -30.00   26
 29  \w     74.00 174.00   1.00    7.00    --  110.40  77.00 -90.00  100
 30  \w     74.00 177.00   1.00    7.00    --  110.40  77.00  30.00  103
 31  \w     74.00 100.00   1.00    7.00    --  110.40  77.00  60.00   26
 32  \w     57.00 120.00   1.00    3.00    --   37.56 178.00 150.00   63
 33  \w     63.00 128.00   1.00    3.00    --   37.56 178.00  60.00   65
 34  \w     34.00  61.00   1.00    3.00    --   68.00  75.00-116.42   27
 35  \w     33.00  60.00   1.00    3.00    --   68.00  76.00-156.95   27
 36  \w     36.00  76.00   1.00    3.00    --   72.00  77.00-177.68   40
 37  \w     74.00 101.00   1.00    7.00    --  110.40  77.00-150.00   27
 38  \w     19.00  44.00   1.00    3.00    --   56.00  81.00-177.70   25
 39  \w     -3.00  23.00   1.00    3.00    --   40.00  96.00-104.08   26
 40  \w     19.00  44.00   1.00    3.00    --   56.00  82.00 -19.02   25
 41  \w     19.00  44.00   1.00    3.00    --   56.00  81.00  12.17   25
 42  \w     26.00  51.00   1.00    3.00    --   60.00  74.00  38.47   25
 43  \w     28.00 146.00   1.00    3.00    --   64.00  75.00  62.88  118
 44  \w     24.00  62.00   1.00    3.00    --   60.00  75.00 131.74   38
 45  \w     19.00  44.00   1.00    3.00    --   56.00  81.00 149.97   25
 46  \w     19.00  44.00   1.00    3.00    --   56.00  80.00  90.98   25
 47  \w      5.00  30.00   1.00    3.00    --   44.00  87.00  89.91   25
 48  \w    -74.00  25.00   1.00    3.00    --  -37.56  77.00-150.00   99
 49  \w   -109.00  -5.00   1.00    3.00    --  -37.56 -57.00 120.00  104
 50  \w   -114.00  -5.00   1.00    3.00    --  -37.56 -57.00   0.00  109
 51  \w   -115.00  -5.00   1.00    3.00    --  -37.56 -57.00-120.00  110
 52  \w     23.00  93.00   1.00    7.00    --  110.40 -94.00 -60.00   70
 53  \w     28.00  98.00   1.00    7.00    --  110.40 -94.00   0.00   70
 54  \w     28.00  96.00   1.00    7.00    --  110.40 -94.00  60.00   68
 55  \w     29.00 113.00   1.00    7.00    --  110.40-111.00 150.00   84
 56  \w     30.00 115.00   1.00    7.00    --  110.40-111.00 -90.00   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_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0350483000
_diffrn_orient_matrix_UB_12      -0.0720441000
_diffrn_orient_matrix_UB_13      -0.0716226000
_diffrn_orient_matrix_UB_21      0.0189041000
_diffrn_orient_matrix_UB_22      0.1091948000
_diffrn_orient_matrix_UB_23      -0.0234687000
_diffrn_orient_matrix_UB_31      0.1514188000
_diffrn_orient_matrix_UB_32      0.0046493000
_diffrn_orient_matrix_UB_33      -0.0072840000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            39775
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.717
_diffrn_reflns_theta_min         3.756
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.764
_exptl_absorpt_correction_T_max  0.447
_exptl_absorpt_correction_T_min  0.103
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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    1.539
_exptl_crystal_description       plate
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.679
_exptl_crystal_size_mid          0.222
_exptl_crystal_size_min          0.126
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         10061
_refine_ls_number_restraints     328
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0864P)^2^+1.1927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1460
_refine_ls_wR_factor_ref         0.1535
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8681
_reflns_number_total             10061
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01747b2.cif
_cod_data_source_block           14
_cod_database_code               7043474
_chemical_oxdiff_formula         'Cr2 N12 P6 F36 C65 h30'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Restrained distances
 N48B-C47B = N48A-C47A
 1.16 with sigma of 0.02
 C47A-C46A = C47B-C46B
 1.45 with sigma of 0.02
 N45B-C44B = N45A-C44A
 1.16 with sigma of 0.02
 C44A-C43A = C44B-C43B
 1.45 with sigma of 0.02
 N54A-C53A = N54B_$2-C53B_$2
 1.16 with sigma of 0.02
 C53B-C52B = C53A_$2-C52A_$2
 1.45 with sigma of 0.02
 N48A-C46A
 2.61 with sigma of 0.04
 N48B-C46B
 2.61 with sigma of 0.04
 N45A-C43A
 2.61 with sigma of 0.04
 C43B-N45B
 2.61 with sigma of 0.04
 N54A-C52A
 2.61 with sigma of 0.04
 N54B-C52B
 2.61 with sigma of 0.04
 F12A-F10A \\sim F12A-F14A \\sim F12A-F13A \\sim F12A-F11A \\sim F10A-F14A
\\sim F10A-F11A \\sim F10A-
 F9A \\sim F14A-F13A \\sim F14A-F9A \\sim F13A-F11A \\sim F11A-F9A
 with sigma of 0.04
 P8A-F12A \\sim P8A-F10A \\sim P8A-F14A \\sim P8A-F13A \\sim P8A-F11A \\sim
P8A-F9A
 with sigma of 0.02
 F9B-F11B \\sim F9B-F13B \\sim F9B-F10B \\sim F9B-F14B \\sim F11B-F13B \\sim
F11B-F10B \\sim F13B-F14B
 \\sim F13B-F12B \\sim F10B-F14B \\sim F14B-F12B
 with sigma of 0.04
 P8B-F9B \\sim P8B-F11B \\sim P8B-F13B \\sim P8B-F10B \\sim P8B-F14B \\sim
P8B-F12B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C46A) = Uanis(C46B)
Uanis(C43A) = Uanis(C43B)
Uanis(N54B) = Uanis(N54A)
Uanis(C53B) = Uanis(C53A)
Uanis(C52B) = Uanis(C52A)
Uanis(F12B) = Uanis(F12A)
4. Rigid body (RIGU) restrains
 N48A, C46A, C47A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N48B, C46B, C47B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N45B, C43B, C44B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N45A, C43A, C44A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N54B, C52B, C53B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N54A, C52A, C53A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P8B, F9B, F10B, F11B, F12B, F13B, F14B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P8A, F9A, F10A, F11A, F12A, F13A, F14A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(N48B)=Sof(C46B)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C47B)=1-FVAR(1)
 Sof(N48A)=Sof(C46A)=Sof(H46D)=Sof(H46E)=Sof(H46F)=Sof(C47A)=FVAR(1)
 Sof(N45B)=Sof(C43B)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C44B)=1-FVAR(2)
 Sof(N45A)=Sof(C43A)=Sof(H43D)=Sof(H43E)=Sof(H43F)=Sof(C44A)=FVAR(2)
 Sof(P8B)=Sof(F9B)=Sof(F10B)=Sof(F11B)=Sof(F12B)=Sof(F13B)=Sof(F14B)=1-FVAR(3)
 Sof(P8A)=Sof(F9A)=Sof(F10A)=Sof(F11A)=Sof(F12A)=Sof(F13A)=Sof(F14A)=FVAR(3)
 Sof(N54B)=Sof(C52B)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C53B)=1-FVAR(4)
 Sof(N54A)=Sof(C52A)=Sof(H52D)=Sof(H52E)=Sof(H52F)=Sof(C53A)=FVAR(4)
6.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C16(H16), C19(H19), C20(H20),
 C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C29(H29), C30(H30),
  C31(H31), C34(H34), C35(H35), C36(H36), C37(H37)
6.b Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C46A(H46D,H46E,H46F), C46B(H46A,H46B,H46C), C43B(H43A,
 H43B,H43C), C43A(H43D,H43E,H43F), C52A(H52D,H52E,H52F), C52B(H52A,H52B,H52C),
 C49(H49A,H49B,H49C)
;
_shelx_shelxl_version_number     2014/7
_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 1.670
_oxdiff_exptl_absorpt_empirical_full_min 0.499