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_4347400
_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         '2(I), B H4 O3, C36 H30 N P2, C2 H3 N'
_chemical_formula_sum            'C38 H37 B I2 N2 O3 P2'
_chemical_formula_weight         896.24
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9964(3)
_cell_length_b                   12.6256(3)
_cell_length_c                   28.4208(10)
_cell_measurement_reflns_used    5161
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.2330
_cell_measurement_theta_min      1.9950
_cell_volume                     3945.8(2)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean 16.2705
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.867
_diffrn_measurement_details
;
  1 omega    9.00   52.00   1.0000  452.2750
omega____ theta____ kappa____ phi______ frames
    -       15.2805  -99.0000 -120.0000 43

  2 omega   38.00   76.00   1.0000  452.2750
omega____ theta____ kappa____ phi______ frames
    -       15.2805   57.0000  -60.0000 38

  3 omega  -51.00   33.00   1.0000  452.2750
omega____ theta____ kappa____ phi______ frames
    -       15.2805  -37.0000  -60.0000 84
;
_diffrn_measurement_device_type  Oxford
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0736
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.867
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            14201
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.797
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.474
_diffrn_reflns_theta_min         1.986
_exptl_absorpt_coefficient_mu    1.712
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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    1.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.043
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details
;
 Flack x determined using 2393 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.024(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         8745
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0241P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0745
_reflns_Friedel_coverage         0.659
_reflns_Friedel_fraction_full    0.930
_reflns_Friedel_fraction_max     0.709
_reflns_number_gt                7076
_reflns_number_total             8745
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00118_si_002.cif
_cod_data_source_block           bk02
_cod_database_code               4347400
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C15(H15), C8(H8), C9(H9), C32(H32), C11(H11), C3(H3), C12(H12),
 C10(H10), C36(H36), C4(H4), C6(H6), C5(H5), C24(H24), C35(H35), C14(H14),
 C30(H30), C28(H28), C27(H27), C22(H22), C20(H20), C29(H29), C23(H23), C17(H17),
  C33(H33), C34(H34), C21(H21), C18(H18), C26(H26), C1A(H1A)
2.b Tetrahedral OH refined with riding coordinates:
 O2(H2A), O3(H3A), O1(H1)
2.c Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C)
;
_shelx_res_checksum              99081
_shelx_hkl_checksum              66266
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'