Tunable carbocation-based redox active ambiphilic ligands: synthesis, coordination and characterization.
Mei, Liangyong; Veleta, José M; Bloch, Jan; Goodman, Hannah J.; Pierce-Navarro, Dominic; Villalobos, Alejandro; Gianetti, Thomas L.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 16095–16105; doi:10.1039/d0dt00419g

data_7703763
_publ_section_title
;
 Tunable carbocation-based redox active ambiphilic ligands: synthesis,
 coordination and characterization.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16095
_journal_page_last               16105
_journal_paper_doi               10.1039/d0dt00419g
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C30 H29 Cl3 Co N2 O4'
_chemical_formula_sum            'C30 H29 Cl3 Co N2 O4'
_chemical_formula_weight         646.83
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-06
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-22 deposited with the CCDC.	2020-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                84.043(3)
_cell_angle_beta                 74.577(3)
_cell_angle_gamma                85.088(3)
_cell_formula_units_Z            2
_cell_length_a                   8.7176(3)
_cell_length_b                   12.5351(4)
_cell_length_c                   13.2082(5)
_cell_measurement_reflns_used    6575
_cell_measurement_temperature    100.00(16)
_cell_measurement_theta_max      28.7660
_cell_measurement_theta_min      2.1940
_cell_volume                     1381.31(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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_environment      N~2~
_diffrn_ambient_temperature      100.00(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0839
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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    -43.00  43.00   1.00    3.00    --  -24.99  57.00 -60.00   86
  2  \w    -94.00   4.00   1.00    3.00    --  -24.99 -77.00 -60.00   98
  3  \w    -25.00  66.00   1.00    3.00    --   25.46 -99.00 -90.00   91
  4  \w    -44.00  54.00   1.00    3.00    --   25.46 -77.00  30.00   98
  5  \w     -3.00  95.00   1.00    3.00    --   25.46  77.00 150.00   98
  6  \w    -25.00  66.00   1.00    3.00    --   25.46 -99.00-120.00   91
  7  \w     34.00 100.00   1.00    3.00    --   25.46 179.00-180.00   66
  8  \w    -99.00 -34.00   1.00    3.00    --  -24.99-179.00  60.00   65
  9  \w      7.00  94.00   1.00    3.00    --   25.46  57.00 -90.00   87
 10  \w      3.00  96.00   1.00    3.00    --   25.46  38.00  30.00   93
 11  \w      7.00  94.00   1.00    3.00    --   25.46  57.00  60.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0248934000
_diffrn_orient_matrix_UB_12      -0.0380385000
_diffrn_orient_matrix_UB_13      -0.0382083000
_diffrn_orient_matrix_UB_21      -0.0716117000
_diffrn_orient_matrix_UB_22      0.0121212000
_diffrn_orient_matrix_UB_23      -0.0158286000
_diffrn_orient_matrix_UB_31      0.0374466000
_diffrn_orient_matrix_UB_32      0.0406789000
_diffrn_orient_matrix_UB_33      -0.0376187000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0643
_diffrn_reflns_av_unetI/netI     0.0646
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30805
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.130
_diffrn_reflns_theta_min         2.194
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.952
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       block
_exptl_crystal_F_000             666
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         7414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0325P)^2^+0.3268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0990
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5574
_reflns_number_total             7414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00419g2.cif
_cod_data_source_block           dpn21-c
_cod_depositor_comments
'Adding full bibliography for 7703758--7703764.cif.'
_cod_database_code               7703763
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C30 H29 N2 O4 Co1 Cl3'
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.847
_reflns_odcompleteness_completeness 87.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C25(H25A,H25B)
2.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C30(H30), C10(H10), C17(H17), C9(H9), C27(H27), C3(H3), C11(H11),
 C28(H28), C18(H18), C2(H2), C1(H1), C19(H19)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C23(H23A,H23B,
 H23C)
;
_shelx_res_checksum              59933
_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 1.107
_oxdiff_exptl_absorpt_empirical_full_min 0.945