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_1529325
_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 N4 P, 3(C F3 O3 S), C2 H3 N'
_chemical_formula_sum            'C41 H51 F9 N5 O9 P S3'
_chemical_formula_weight         1056.01
_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                88.2712(4)
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_cell_angle_gamma                88.0482(4)
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_cell_length_b                   14.5562(5)
_cell_length_c                   14.5880(5)
_cell_measurement_reflns_used    8344
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.42
_cell_measurement_theta_min      2.23
_cell_volume                     2440.47(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
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_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
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_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
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_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         26.823
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_exptl_absorpt_coefficient_mu    0.276
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9222
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            yellow
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_exptl_crystal_description       block
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_exptl_crystal_size_min          0.068
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         10419
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0633P)^2^+1.6415P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1398
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8068
_reflns_number_total             10419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02423d2.cif
_cod_data_source_block           vic1509
_cod_depositor_comments
'Adding full bibliography for 1529324--1529330.cif.'
_cod_database_code               1529325
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.896
_shelx_estimated_absorpt_t_max   0.982
_shelx_res_checksum              47480