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_7043470
_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         'C17 H17 Cl3 Cr N5'
_chemical_formula_sum            'C17 H17 Cl3 Cr N5'
_chemical_formula_weight         449.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-09-20
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2017-04-05 deposited with the CCDC.
2017-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.140(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2232(4)
_cell_length_b                   14.8231(6)
_cell_length_c                   13.6125(5)
_cell_measurement_reflns_used    3624
_cell_measurement_temperature    180.15
_cell_measurement_theta_max      73.4350
_cell_measurement_theta_min      4.4260
_cell_volume                     1850.38(13)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      180.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4679
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.967
_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     81.00 171.00   1.00    1.50    --  110.40  45.00-120.00   90
  2  \w    105.00 142.00   1.00    1.50    --  110.40 111.00-180.00   37
  3  \w    104.00 130.00   1.00    1.50    --  110.40  91.00 -47.00   26
  4  \w    121.00 171.00   1.00    1.50    --  110.40 111.00  30.00   50
  5  \w    100.00 178.00   1.00    1.50    --  110.40 111.00  60.00   78
  6  \w     57.00 143.00   1.00    1.50    --  110.40 -30.00-120.00   86
  7  \w     23.00 109.00   1.00    1.50    --  110.40 -94.00-180.00   86
  8  \w     11.00  79.00   1.00    1.00    --   37.69 -99.00-180.00   68
  9  \w    -42.00 -16.00   1.00    1.00    --  -37.69 -38.00   0.00   26
 10  \w    -72.00 -41.00   1.00    1.00    --  -37.69 178.00 -60.00   31
 11  \w   -128.00 -99.00   1.00    1.00    --  -37.69 178.00 -60.00   29
 12  \w   -117.00 -44.00   1.00    1.00    --  -37.69 -38.00   0.00   73
 13  \w   -128.00 -65.00   1.00    1.00    --  -37.69-178.00-120.00   63
;
_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      -0.1396471000
_diffrn_orient_matrix_UB_12      0.0221801000
_diffrn_orient_matrix_UB_13      0.0478962000
_diffrn_orient_matrix_UB_21      0.0638464000
_diffrn_orient_matrix_UB_22      0.0926498000
_diffrn_orient_matrix_UB_23      0.0326621000
_diffrn_orient_matrix_UB_31      -0.0676621000
_diffrn_orient_matrix_UB_32      0.0417997000
_diffrn_orient_matrix_UB_33      -0.0979657000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6966
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.718
_diffrn_reflns_theta_min         4.424
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.171
_exptl_absorpt_correction_T_max  0.505
_exptl_absorpt_correction_T_min  0.291
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       block
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.343
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.063
_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     237
_refine_ls_number_reflns         3620
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0517P)^2^+0.8165P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3221
_reflns_number_total             3620
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01747b2.cif
_cod_data_source_block           15
_cod_database_code               7043470
_chemical_oxdiff_formula         'C17 H17 Cl3 Cr1 N5'
_reflns_odcompleteness_completeness 99.74
_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.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C13(H13), C14(H14), C15(H15), C18(H18),
 C19(H19), C20(H20), C21(H21)
2.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C17(H17A,H17B,H17C)
;
_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 1.409
_oxdiff_exptl_absorpt_empirical_full_min 0.733