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_7703758
_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         'B F4, C30 H29 N2 O4, 0.05(C H2 Cl2)'
_chemical_formula_sum            'C30.05 H29.1 B Cl0.1 F4 N2 O4'
_chemical_formula_weight         572.61
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-09-09
_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                90
_cell_angle_beta                 98.088(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8254(5)
_cell_length_b                   13.2164(4)
_cell_length_c                   15.3735(5)
_cell_measurement_reflns_used    7779
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.9770
_cell_measurement_theta_min      2.0310
_cell_volume                     2781.14(16)
_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    'ShelXS (Sheldrick, 2008)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.926
_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    -49.00  48.00   1.00   15.02    --  -20.71  77.00  30.00   97
  2  \w    -39.00  48.00   1.00   15.02    --  -20.71  57.00 -60.00   87
  3  \w    -25.00  20.00   1.00   15.02    --  -20.71 -99.00  60.00   45
  4  \w    -25.00  20.00   1.00   15.02    --  -20.71 -99.00 -90.00   45
  5  \w    -25.00  20.00   1.00   15.02    --  -20.71 -99.00-180.00   45
  6  \w    -50.00  92.00   1.00   15.02    --   21.18   0.00 -60.00  142
  7  \w     -1.00  92.00   1.00   15.02    --   21.18  38.00-180.00   93
  8  \w    -49.00  43.00   1.00   15.02    --   21.18 -38.00 150.00   92
;
_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      0.0209429000
_diffrn_orient_matrix_UB_12      0.0030937000
_diffrn_orient_matrix_UB_13      0.0447311000
_diffrn_orient_matrix_UB_21      -0.0473892000
_diffrn_orient_matrix_UB_22      0.0031365000
_diffrn_orient_matrix_UB_23      0.0125207000
_diffrn_orient_matrix_UB_31      -0.0016267000
_diffrn_orient_matrix_UB_32      -0.0535034000
_diffrn_orient_matrix_UB_33      0.0033057000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            42410
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.857
_diffrn_reflns_theta_min         1.856
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92404
_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            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         8104
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+1.2971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1179
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5653
_reflns_number_total             8104
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00419g2.cif
_cod_data_source_block           hg27-a
_cod_depositor_comments
'Adding full bibliography for 7703758--7703764.cif.'
_cod_original_cell_volume        2781.15(16)
_cod_original_formula_sum        'C30.05 H29.10 B Cl0.10 F4 N2 O4'
_cod_database_code               7703758
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C30.1 H29.1 N2 O4 B1 F4 Cl0.1'
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.977
_reflns_odcompleteness_completeness 99.96
_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. Restrained distances
 Cl1-C31 = Cl2-C31
 1.771 with sigma of 0.01
 Cl1-Cl2
 2.916 with sigma of 0.03
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim C31: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Rigid body (RIGU) restrains
 Cl1, Cl2, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Cl1)=Sof(Cl2)=Sof(C31)=Sof(H31A)=Sof(H31B)=0.5*FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C25(H25A,H25B), C31(H31A,H31B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C10(H10), C11(H11), C17(H17), C2(H2), C9(H9), C27(H27), C18(H18),
 C1(H1), C19(H19), C28(H28), C29(H29), C30(H30)
6.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C)
;
_shelx_res_checksum              89072
_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 1.106
_oxdiff_exptl_absorpt_empirical_full_min 0.869