Polyfluorinated carba-closo-dodecaboranes with amino and ammonio substituents bonded to boron.
Konieczka, Szymon Z.; Drisch, Michael; Edkins, Katharina; Hailmann, Michael; Finze, Maik; Dalton transactions (Cambridge, England : 2003) 44 (2015) 19576–19586; doi:10.1039/c5dt02055g

data_7035673
_publ_section_title
;
 Polyfluorinated carba-closo-dodecaboranes with amino and ammonio
 substituents bonded to boron.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19576
_journal_page_last               19586
_journal_paper_doi               10.1039/c5dt02055g
_journal_volume                  44
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C H4 B11 F10 N, 0.5(H2 O)'
_chemical_formula_sum            'C H5 B11 F10 N O0.5'
_chemical_formula_weight         348.11
_space_group_crystal_system      orthorhombic
_space_group_IT_number           37
_space_group_name_Hall           'C 2 -2c'
_space_group_name_H-M_alt        'C c c 2'
_symmetry_space_group_name_Hall  'C 2 -2c'
_symmetry_space_group_name_H-M   'C c c 2'
_atom_sites_solution_primary     direct
_audit_creation_date             2013-04-30
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_audit_update_record
;
2015-05-19 deposited with the CCDC.
2015-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   14.684(4)
_cell_length_b                   22.575(7)
_cell_length_c                   14.269(4)
_cell_measurement_reflns_used    7045
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.70
_cell_measurement_theta_min      2.19
_cell_volume                     4730(2)
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.9996
_diffrn_measured_fraction_theta_max 0.9996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'double mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31184
_diffrn_reflns_theta_full        25.9988
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.65
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.216
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1303 before and 0.0682 after correction.
The Ratio of minimum to maximum transmission is 0.8919.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.9543
_exptl_crystal_description       plate
_exptl_crystal_F_000             2674.9061
_exptl_crystal_preparation       'soaked in perfluoro polyether oil'
_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.077
_refine_diff_density_max         0.3410
_refine_diff_density_min         -0.2430
_refine_diff_density_rms         0.0649
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.1(6)
_refine_ls_d_res_high            0.8107
_refine_ls_d_res_low             12.3092
_refine_ls_goodness_of_fit_ref   1.0613
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    16
_refine_ls_number_parameters     426
_refine_ls_number_reflns         4659
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0613
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+0.5304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0957
_reflns_Friedel_coverage         0.999
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              27
_reflns_limit_k_min              -27
_reflns_limit_l_max              17
_reflns_limit_l_min              -17
_reflns_number_gt                4010
_reflns_number_total             4659
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5dt02055g2.cif
_cod_data_source_block           13S005
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7035673--7035677.cif.
;
_cod_database_code               7035673
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Riding coordinates:
 O2W(H2W), O1W(H1W)
2.b Idealised Me refined as rotating group:
 N1B(H1Ba,H1Bb,H1Bc), N1A(H1Aa,H1Ab,H1Ac)
2.c Boron cage BH refined with riding coordinates:
 C1A(H1A), C1B(H1B)
;