Tuning the electrochemical potential of perfunctionalized dodecaborate clusters through vertex differentiation.
Wixtrom, Alex I.; Parvez, Zeeshan A.; Savage, Miles D.; Qian, Elaine A.; Jung, Dahee; Khan, Saeed I.; Rheingold, Arnold L.; Spokoyny, Alexander M.; Chemical communications (Cambridge, England) 54 (2018) 5867–5870; doi:10.1039/c8cc03477j

data_7121657
_publ_section_title
;
 Tuning the electrochemical potential of perfunctionalized dodecaborate
 clusters through vertex differentiation.
;
_journal_issue                   46
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5867
_journal_page_last               5870
_journal_paper_doi               10.1039/c8cc03477j
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C77 H22 B12 F55 N O13, C16 H36 N'
_chemical_formula_sum            'C93 H58 B12 F55 N2 O13'
_chemical_formula_weight         2586.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-12-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-29 deposited with the CCDC.
2018-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                110.4400(10)
_cell_angle_beta                 91.6990(10)
_cell_angle_gamma                97.1390(10)
_cell_formula_units_Z            4
_cell_length_a                   14.1250(3)
_cell_length_b                   27.2616(5)
_cell_length_c                   29.4644(6)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.80
_cell_measurement_theta_min      2.23
_cell_volume                     10516.5(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2016)'
_computing_data_collection       'APEX3 v2016.1-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8.258
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_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  0.0454
_diffrn_reflns_av_unetI/netI     0.0762
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            79433
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.292
_diffrn_reflns_theta_min         1.273
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_T_max  0.6462
_exptl_absorpt_correction_T_min  0.6188
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0836 before and 0.0421 after correction. The Ratio of minimum to maximum transmission is 0.9576. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_description       block
_exptl_crystal_F_000             5156
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.257
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3184
_refine_ls_number_reflns         38080
_refine_ls_number_restraints     3236
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1376
_refine_ls_R_factor_gt           0.0857
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1200P)^2^+32.2443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2226
_refine_ls_wR_factor_ref         0.2595
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23259
_reflns_number_total             38080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc03477j2.cif
_cod_data_source_block           spok88_0m_a_sq
_cod_depositor_comments
'Adding full bibliography for 7121656--7121657.cif.'
_cod_database_code               7121657
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.947
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C108-C109
 1.54 with sigma of 0.001
 C112-C113
 1.54 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C109) = Uanis(C107)
Uanis(C111) = Uanis(C113)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C106(0.5) H10O(0.5) H10P(0.5) C107(0.5) H10Q(0.5) H10R(0.5)
 C108(0.5) H10S(0.5) H10T(0.5) H10U(0.5) C109(0.5) H10V(0.5) H10W(0.5)
 C110(0.5) H11A(0.5) H11B(0.5) C111(0.5) H11C(0.5) H11D(0.5) C112(0.5)
 H11E(0.5) H11F(0.5) C113(0.5) H11G(0.5) H11H(0.5) H11I(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C15(H15A,H15B), C28(H28A,H28B), C35(H35A,H35B),
 C36(H36A,H36B), C43(H43A,H43B), C50(H50A,H50B), C57(H57A,H57B), C64(H64A,H64B),
  C71(H71A,H71B), C1'(H1'A,H1'B), C8'(H8'A,H8'B), C15'(H15C,H15D), C28'(H28C,
 H28D), C35'(H35C,H35D), C36'(H36C,H36D), C43'(H43C,H43D), C50'(H50C,H50D),
 C57'(H57C,H57D), C64'(H64C,H64D), C71'(H71C,H71D), C78(H78A,H78B), C79(H79A,
 H79B), C80(H80A,H80B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B),
 C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B), C90(H90A,H90B), C91(H91A,H91B),
  C92(H92A,H92B), C94(H94A,H94B), C95(H95A,H95B), C96(H96A,H96B), C98(H98A,
 H98B), C99(H99A,H99B), C100(H10A,H10B), C102(H10F,H10G), C103(H10H,H10I),
 C104(H10J,H10K), C106(H10O,H10P), C107(H10Q,H10R), C109(H10V,H10W), C110(H11A,
 H11B), C111(H11C,H11D), C112(H11E,H11F)
6.b Idealised Me refined as rotating group:
 C81(H81A,H81B,H81C), C85(H85A,H85B,H85C), C89(H89A,H89B,H89C), C93(H93A,H93B,
 H93C), C97(H97A,H97B,H97C), C101(H10C,H10D,H10E), C105(H10L,H10M,H10N),
 C108(H10S,H10T,H10U), C113(H11G,H11H,H11I)
;
_shelx_res_checksum              32210
_shelx_fab_checksum              88186
_olex2_submission_special_instructions 'No special instructions were received'