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_7703764
_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 N2 Ni O4'
_chemical_formula_sum            'C30 H29 Cl3 N2 Ni O4'
_chemical_formula_weight         646.61
_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             2019-09-03
_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                83.920(3)
_cell_angle_beta                 74.506(3)
_cell_angle_gamma                84.865(3)
_cell_formula_units_Z            2
_cell_length_a                   8.6529(3)
_cell_length_b                   12.5362(4)
_cell_length_c                   13.2372(5)
_cell_measurement_reflns_used    10086
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.5030
_cell_measurement_theta_min      2.3800
_cell_volume                     1373.12(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.16b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.16b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.16b (Rigaku OD, 2018)'
_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(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0839
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.917
_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 -3.00 1.00 2.50 -- -20.71 134.00 102.00 78 2 \w -25.00 20.00 1.00 2.50 -- -20.71 -99.00 30.00 45 3 \w -25.00 20.00 1.00 2.50 -- -20.71 -99.00-150.00 45 4 \w -25.00 20.00 1.00 2.50 -- -20.71 -99.00 -60.00 45 5 \w -95.00 -32.00 1.00 2.50 -- -20.71 179.00 -30.00 63 6 \w -95.00 -32.00 1.00 2.50 -- -20.71 179.00-120.00 63 7 \w -49.00 43.00 1.00 2.50 -- 21.18 -38.00-150.00 92 8 \w -50.00 92.00 1.00 2.50 -- 21.18 0.00 60.00 142 9 \w -89.00 -2.00 1.00 2.50 -- -20.71 -57.00-150.00 87 10 \w -25.00 20.00 1.00 2.50 -- -20.71 -99.00 -90.00 45 11 \w -82.00 -4.00 1.00 2.50 -- -20.71 136.00 -79.00 78 12 \w -59.00 52.00 1.00 2.50 -- -20.71 19.00 30.00 111 13 \w 3.00 90.00 1.00 2.50 -- 21.18 57.00 90.00 87 14 \w 3.00 90.00 1.00 2.50 -- 21.18 57.00-180.00 87 15 \w -25.00 18.00 1.00 2.50 -- -20.71 -99.00 -30.00 43'
_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      0.0121852000
_diffrn_orient_matrix_UB_12      -0.0538559000
_diffrn_orient_matrix_UB_13      0.0202992000
_diffrn_orient_matrix_UB_21      -0.0294889000
_diffrn_orient_matrix_UB_22      0.0156805000
_diffrn_orient_matrix_UB_23      0.0519826000
_diffrn_orient_matrix_UB_31      -0.0790405000
_diffrn_orient_matrix_UB_32      -0.0102259000
_diffrn_orient_matrix_UB_33      -0.0006066000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       12
_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            36350
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.915
_diffrn_reflns_theta_min         2.191
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.039
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.40.16b (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_description       needle
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         7966
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0460P)^2^+0.4135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.1067
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6386
_reflns_number_total             7966
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00419g2.cif
_cod_data_source_block           m-2-111-1c
_cod_depositor_comments
'Adding full bibliography for 7703758--7703764.cif.'
_cod_database_code               7703764
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Ni1 Cl3 N2 O4 C30 H29'
_shelx_estimated_absorpt_t_max   0.804
_shelx_estimated_absorpt_t_min   0.658
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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:
 C30(H30), C11(H11), C19(H19), C9(H9), C27(H27), C29(H29), C10(H10), C18(H18),
 C3(H3), C28(H28), C2(H2), C1(H1), C17(H17)
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C)
;
_shelx_res_checksum              16852
_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 1.305
_oxdiff_exptl_absorpt_empirical_full_min 0.845