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_7703759
_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         'C31 H30 N3 O2, B F4'
_chemical_formula_sum            'C32 H31 B F4 N2 O2'
_chemical_formula_weight         562.40
_chemical_name_systematic        mly135
_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     dual
_audit_creation_date             2019-10-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 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                 110.983(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.823(3)
_cell_length_b                   21.139(5)
_cell_length_c                   12.359(3)
_cell_measurement_reflns_used    4901
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.831
_cell_measurement_theta_min      2.23
_cell_volume                     2640.1(12)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23832
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.742
_diffrn_reflns_theta_min         1.927
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0557 before and 0.0470 after correction. The Ratio of minimum to maximum transmission is 0.8837. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'metallic dark green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       plate
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         4986
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0766P)^2^+2.1309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1458
_refine_ls_wR_factor_ref         0.1600
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3704
_reflns_number_total             4986
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00419g2.cif
_cod_data_source_block           mo_mly135helicene_0m
_cod_depositor_comments
'Adding full bibliography for 7703758--7703764.cif.'
_cod_original_cell_volume        2640.0(11)
_cod_database_code               7703759
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.972
_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:
 C00K(H00A,H00B), C00P(H00C,H00D), C00Q(H00E,H00F), C00W(H00K,H00P)
2.b Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00L(H00L), C00M(H00M), C00N(H00N), C00O(H00O), C00R(H00R),
 C00S(H00S), C00X(H00X), C00Z(H00Z), C010(H010), C012(H012), C013(H013),
 C014(H014)
2.c Idealised Me refined as rotating group:
 C00V(H00G,H00I,H00J), C00Y(H00Q,H00T,H00U), C011(H01A,H01B,H01C)
;
_shelx_res_checksum              25995
_olex2_submission_special_instructions 'No special instructions were received'