Theoretical and Synthetic Study on the Existence, Structures, and Bonding of the Halide-Bridged [B2X7](-) (X = F, Cl, Br, I) Anions.
Bertocco, Philipp; Bolli, Christoph; Correia Bicho, Bruno A.; Jenne, Carsten; Erken, Berrin; Laitinen, Risto S.; Seeger, Helene A.; Takaluoma, Teemu T.; Inorganic chemistry 55 (2016) 3599–3604; doi:10.1021/acs.inorgchem.6b00118

data_4347401
_publ_section_title
;
 Theoretical and Synthetic Study on the Existence, Structures, and Bonding
 of the Halide-Bridged [B2X7](-) (X = F, Cl, Br, I) Anions.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3599
_journal_page_last               3604
_journal_paper_doi               10.1021/acs.inorgchem.6b00118
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C36 H30 N P2, C H2 Cl2, Cl2 H'
_chemical_formula_sum            'C37 H33 Cl4 N P2'
_chemical_formula_weight         695.38
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-10-05
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90.314(3)
_cell_angle_beta                 93.380(3)
_cell_angle_gamma                94.617(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4626(4)
_cell_length_b                   10.5499(4)
_cell_length_c                   16.9579(4)
_cell_measurement_reflns_used    8295
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.5730
_cell_measurement_theta_min      1.9430
_cell_volume                     1684.38(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 16.2705
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.855
_diffrn_measurement_details
;
  1 omega   28.00   64.00   1.0000   50.3700
omega____ theta____ kappa____ phi______ frames
    -       21.6327  -99.0000  -30.0000 36

  2 omega   27.00   57.00   1.0000   50.3700
omega____ theta____ kappa____ phi______ frames
    -       21.6327   57.0000  150.0000 30

  3 omega  -77.00   -8.00   1.0000   50.3700
omega____ theta____ kappa____ phi______ frames
    -      -23.3515  -57.0000 -180.0000 69

  4 omega  -93.00  -53.00   1.0000   50.3700
omega____ theta____ kappa____ phi______ frames
    -      -23.3515  -77.0000 -180.0000 40

  5 omega  -37.00  -10.00   1.0000   50.3700
omega____ theta____ kappa____ phi______ frames
    -      -23.3515  -77.0000 -180.0000 27

  6 omega  -46.00   48.00   1.0000   50.3700
omega____ theta____ kappa____ phi______ frames
    -      -23.3515   37.0000  -30.0000 94

  7 omega  -91.00    7.00   1.0000   50.3700
omega____ theta____ kappa____ phi______ frames
    -      -23.3515  -77.0000   60.0000 98

  8 omega  -61.00  -32.00   1.0000   50.3700
omega____ theta____ kappa____ phi______ frames
    -      -23.3515  178.0000  -90.0000 29
;
_diffrn_measurement_device_type  Oxford
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0639269000
_diffrn_orient_matrix_UB_12      -0.0077846000
_diffrn_orient_matrix_UB_13      0.0228153000
_diffrn_orient_matrix_UB_21      0.0050566000
_diffrn_orient_matrix_UB_22      0.0653882000
_diffrn_orient_matrix_UB_23      0.0106538000
_diffrn_orient_matrix_UB_31      -0.0395386000
_diffrn_orient_matrix_UB_32      -0.0146295000
_diffrn_orient_matrix_UB_33      0.0334925000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.855
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16114
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.855
_diffrn_reflns_theta_full        28.300
_diffrn_reflns_theta_max         31.014
_diffrn_reflns_theta_min         1.937
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.475
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         9210
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+0.8252P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0896
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7751
_reflns_number_total             9210
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00118_si_002.cif
_cod_data_source_block           hs04
_cod_database_code               4347401
_chemical_oxdiff_formula         C36H30P2N1B1Cl4
_reflns_odcompleteness_completeness 99.99
_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
2.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
;
_shelx_res_checksum              21295
_shelx_hkl_checksum              77269
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'