Bipyridine complexes of E3+(E = P, As, Sb, Bi): strong Lewis acids, sources of E(OTf)3and synthons for EIand EVcations
Chitnis, Saurabh S.; Robertson, Alasdair P. M.; Burford, Neil; Patrick, Brian O.; McDonald, Robert; Ferguson, Michael J.; Chem. Sci. 6 (2015) 6545–; doi:10.1039/C5SC02423D

data_1529326
_publ_section_title
;
 Bipyridine complexes of E3+(E = P, As, Sb, Bi): strong Lewis acids,
 sources of E(OTf)3and synthons for EIand EVcations
;
_journal_issue                   11
_journal_name_full               'Chem. Sci.'
_journal_page_first              6545
_journal_paper_doi               10.1039/C5SC02423D
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C36 H48 As N4, 3(C F3 O3 S), 2.833(C2 H3 N)'
_chemical_formula_sum            'C44.67 H56.5 As F9 N6.83 O9 S3'
_chemical_formula_weight         1175.23
_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_method           SHELXL-2014/7
_audit_update_record
;
2015-07-05 deposited with the CCDC.
2015-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                93.9090(6)
_cell_angle_beta                 101.3392(6)
_cell_angle_gamma                99.3536(6)
_cell_formula_units_Z            6
_cell_length_a                   15.0217(6)
_cell_length_b                   18.4434(8)
_cell_length_c                   31.1243(13)
_cell_measurement_reflns_used    9657
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.22
_cell_measurement_theta_min      2.28
_cell_volume                     8297.5(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            38133
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.585
_diffrn_reflns_theta_min         0.671
_exptl_absorpt_coefficient_mu    0.814
_exptl_absorpt_correction_T_max  0.745554
_exptl_absorpt_correction_T_min  0.684427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS 2012/1 (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3638
_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.148
_refine_diff_density_max         1.035
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1983
_refine_ls_number_reflns         38133
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0598P)^2^+2.8233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1208
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27925
_reflns_number_total             38133
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02423d2.cif
_cod_data_source_block           vic1503
_cod_depositor_comments
'Adding full bibliography for 1529324--1529330.cif.'
_cod_original_formula_sum        'C44.67 H56.50 As F9 N6.83 O9 S3'
_cod_database_code               1529326
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.788
_shelx_estimated_absorpt_t_max   0.889
_shelx_res_checksum              47561