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_4347402
_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, B F4'
_chemical_formula_sum            'C36 H30 B F4 N P2'
_chemical_formula_weight         625.36
_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
_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
_cell_angle_beta                 112.707(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.0162(8)
_cell_length_b                   27.5493(8)
_cell_length_c                   16.1105(6)
_cell_measurement_reflns_used    7662
_cell_measurement_temperature    109.8(5)
_cell_measurement_theta_max      29.2400
_cell_measurement_theta_min      2.0800
_cell_volume                     6148.1(5)
_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
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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)'
_diffrn_ambient_temperature      109.8(5)
_diffrn_detector_area_resol_mean 16.2705
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.822
_diffrn_measurement_details
;
  1 omega   22.00   78.00   1.0000  136.6200
omega____ theta____ kappa____ phi______ frames
    -       17.8225 -130.0000  -36.0000 56

  2 omega   -4.00   24.00   1.0000  136.6200
omega____ theta____ kappa____ phi______ frames
    -       17.8225  -99.0000 -120.0000 28

  3 omega  -21.00   48.00   1.0000  136.6200
omega____ theta____ kappa____ phi______ frames
    -      -19.3850   57.0000   90.0000 69

  4 omega  -53.00   14.00   1.0000  136.6200
omega____ theta____ kappa____ phi______ frames
    -      -19.3850   19.0000   90.0000 67
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0511208000
_diffrn_orient_matrix_UB_12      -0.0005204000
_diffrn_orient_matrix_UB_13      0.0172741000
_diffrn_orient_matrix_UB_21      -0.0006848000
_diffrn_orient_matrix_UB_22      -0.0251903000
_diffrn_orient_matrix_UB_23      0.0088323000
_diffrn_orient_matrix_UB_31      -0.0014942000
_diffrn_orient_matrix_UB_32      -0.0052997000
_diffrn_orient_matrix_UB_33      -0.0436672000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.822
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26711
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.822
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.443
_diffrn_reflns_theta_min         1.645
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.193
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89389
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       block
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         13992
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+1.4655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1102
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10946
_reflns_number_total             13992
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00118_si_002.cif
_cod_data_source_block           bb06
_cod_database_code               4347402
_chemical_oxdiff_formula         C36H30P2N1B1F4
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C60(H60), C70(H70), C20(H20), C26(H26), C38(H38), C50(H50), C12(H12),
 C68(H68), C2(H2), C9(H9), C42(H42), C66(H66), C30(H30), C41(H41), C62(H62),
 C44(H44), C39(H39), C69(H69), C28(H28), C63(H63), C72(H72), C18(H18), C48(H48),
  C65(H65), C22(H22), C45(H45), C32(H32), C71(H71), C10(H10), C8(H8), C36(H36),
 C14(H14), C11(H11), C33(H33), C15(H15), C51(H51), C52(H52), C56(H56), C21(H21),
  C54(H54), C47(H47), C29(H29), C4(H4), C6(H6), C59(H59), C5(H5), C64(H64),
 C40(H40), C27(H27), C24(H24), C58(H58), C46(H46), C23(H23), C16(H16), C34(H34),
  C35(H35), C57(H57), C17(H17), C53(H53)
;
_shelx_res_checksum              54756
_shelx_hkl_checksum              37913
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'