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_7703761
_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         'C29 H27 Cl3 N2 Ni O4, 0.5(C4 H8 O)'
_chemical_formula_sum            'C31 H31 Cl3 N2 Ni O4.5'
_chemical_formula_weight         668.64
_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             2019-09-08
_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                110.441(3)
_cell_angle_beta                 98.644(3)
_cell_angle_gamma                101.914(2)
_cell_formula_units_Z            2
_cell_length_a                   7.5471(2)
_cell_length_b                   13.4245(4)
_cell_length_c                   16.5205(5)
_cell_measurement_reflns_used    6147
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.2130
_cell_measurement_theta_min      2.5390
_cell_volume                     1488.78(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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0839
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.877
_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 -93.00 17.00 0.50 5.00 -- -20.55 -19.00 150.00 220 2 \w -25.00 20.00 0.50 5.00 -- -20.55 -99.00 90.00 90 3 \w -25.00 20.00 0.50 5.00 -- -20.55 -99.00 -90.00 90 4 \w -17.00 94.00 0.50 5.00 -- 21.18 19.00-180.00 222 5 \w 34.00 95.00 0.50 5.00 -- 21.18 179.00 90.00 122 6 \w -47.00 40.00 0.50 5.00 -- 21.18 -57.00 90.00 174 7 \w -48.00 50.00 0.50 5.00 -- 21.18 -77.00-180.00 196'
_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      0.0493179000
_diffrn_orient_matrix_UB_12      0.0567386000
_diffrn_orient_matrix_UB_13      0.0238352000
_diffrn_orient_matrix_UB_21      0.0080282000
_diffrn_orient_matrix_UB_22      -0.0078339000
_diffrn_orient_matrix_UB_23      0.0405484000
_diffrn_orient_matrix_UB_31      0.0854820000
_diffrn_orient_matrix_UB_32      -0.0129766000
_diffrn_orient_matrix_UB_33      -0.0042874000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20068
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.863
_diffrn_reflns_theta_min         2.546
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.963
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84855
_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    1.492
_exptl_crystal_description       plate
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         8217
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0344P)^2^+0.2465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1071
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6410
_reflns_number_total             8217
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00419g2.cif
_cod_data_source_block           m-2-144-2n
_cod_depositor_comments
'Adding full bibliography for 7703758--7703764.cif.'
_cod_original_cell_volume        1488.78(8)
_cod_original_formula_sum        'C31 H31 Cl3 N2 Ni O4.50'
_cod_database_code               7703761
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Ni1 Cl3 N2 O4.5 C31 H31'
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.596
_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
 C30-C31 \\sim C31-C32 \\sim C32-C33
 with sigma of 0.02
 O5-C30 \\sim O5-C33
 with sigma of 0.02
 O5-C31 \\sim O5-C32
 with sigma of 0.04
 C31-C33 \\sim C30-C32
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 C31, H31A, H31B, C32, C30, H32A, H32B, C33, O5, H30A, H30B, H33A, H33B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C31(0.5) H31A(0.5) H31B(0.5) C32(0.5) H32A(0.5) H32B(0.5) C33(0.5)
 H33A(0.5) H33B(0.5) O5(0.5) C30(0.5) H30A(0.5) H30B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C30(H30A,H30B)
5.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C28(H28), C27(H27), C26(H26), C19(H19), C17(H17), C11(H11), C1(H1),
 C18(H18), C2(H2), C9(H9), C3(H3), C10(H10)
5.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C14(H14A,H14B,
 H14C)
;
_shelx_res_checksum              85310
_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 1.127
_oxdiff_exptl_absorpt_empirical_full_min 0.866