#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:04:11 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179091 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/53/4305382.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4305382
loop_
_publ_author_name
'Gemma Barberà'
'Albert Vaca'
'Francesc Teixidor'
'Reijo Sillanpää'
'Raikko Kivekäs'
'Clara Viñas'
_publ_contact_author
;
     Prof. Clara Viñas
     Institute of Material Sciences 
     Campus UAB
     E-08193 Bellaterra
     Spain
;
_publ_contact_author_email       clara@icmab.es
_publ_contact_author_fax         '+34 93 5805729'
_publ_contact_author_phone       '+34 93 5801853'
_publ_section_title
;
Designed Synthesis of New ortho-Carborane Derivatives: from Mono- to
Polysubstituted Frameworks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7309
_journal_page_last               7316
_journal_paper_doi               10.1021/ic800362z
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C4 H16 B10'
_chemical_formula_sum            'C4 H16 B10'
_chemical_formula_weight         172.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.220(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8528(7)
_cell_length_b                   6.8281(3)
_cell_length_c                   11.5332(6)
_cell_measurement_reflns_used    1721
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.91
_cell_volume                     1066.70(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Mok\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3110
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.34
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.046
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.073
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     65
_refine_ls_number_reflns         934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0942
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 calc w=1/[σ²(Fo²)+(0.1857P)²+1.3403P] where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2524
_refine_ls_wR_factor_ref         0.2678
_reflns_number_gt                728
_reflns_number_total             934
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800362z-file001_3.cif
_cod_data_source_block           3,6-Me2-1,2-C2B10H10
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4305382
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.00092(18) 0.0260(4) 0.8204(2) 0.0208(8) Uani 1 d . . .
H1 H 0.0016 -0.1150 0.8703 0.025 Uiso 1 calc R . .
B3 B -0.1098(2) 0.0856(4) 0.6944(3) 0.0230(8) Uani 1 d . . .
B4 B -0.0641(2) 0.2165(4) 0.8420(3) 0.0236(8) Uani 1 d . . .
H4 H -0.1056 0.2143 0.9041 0.028 Uiso 1 calc R . .
B7 B -0.0675(2) 0.2161(4) 0.5917(3) 0.0237(8) Uani 1 d . . .
H7 H -0.1115 0.2136 0.4862 0.028 Uiso 1 calc R . .
B8 B -0.1071(2) 0.3452(4) 0.6958(3) 0.0261(9) Uani 1 d . . .
H8 H -0.1774 0.4315 0.6600 0.031 Uiso 1 calc R . .
B9 B 0.0011(2) 0.4254(4) 0.8277(3) 0.0277(9) Uani 1 d . . .
H9 H 0.0019 0.5649 0.8793 0.033 Uiso 1 calc R . .
C3 C -0.1975(2) -0.0652(5) 0.6507(3) 0.0361(9) Uani 1 d . . .
H3A H -0.1924 -0.1465 0.7232 0.054 Uiso 1 calc R . .
H3B H -0.1944 -0.1489 0.5834 0.054 Uiso 1 calc R . .
H3C H -0.2604 0.0057 0.6183 0.054 Uiso 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 C1 B7 111.56(18) 2_556 2_556 ?
C1 C1 B4 111.85(17) 2_556 . ?
B7 C1 B4 63.41(16) 2_556 . ?
C1 C1 B3 62.52(18) 2_556 . ?
B7 C1 B3 116.16(19) 2_556 . ?
B4 C1 B3 62.86(16) . . ?
C1 C1 B3 62.25(17) 2_556 2_556 ?
B7 C1 B3 62.77(17) 2_556 2_556 ?
B4 C1 B3 116.24(19) . 2_556 ?
B3 C1 B3 117.45(18) . 2_556 ?
C1 C1 H1 120.7 2_556 . ?
B7 C1 H1 118.1 2_556 . ?
B4 C1 H1 117.9 . . ?
B3 C1 H1 115.9 . . ?
B3 C1 H1 116.0 2_556 . ?
C3 B3 C1 119.3(2) . . ?
C3 B3 C1 119.7(2) . 2_556 ?
C1 B3 C1 55.23(16) . 2_556 ?
C3 B3 B8 132.1(2) . . ?
C1 B3 B8 102.51(19) . . ?
C1 B3 B8 102.49(19) 2_556 . ?
C3 B3 B7 125.7(2) . . ?
C1 B3 B7 101.64(19) . . ?
C1 B3 B7 57.30(15) 2_556 . ?
B8 B3 B7 59.69(15) . . ?
C3 B3 B4 124.9(2) . . ?
C1 B3 B4 57.49(15) . . ?
C1 B3 B4 101.82(18) 2_556 . ?
B8 B3 B4 59.63(15) . . ?
B7 B3 B4 106.36(19) . . ?
C1 B4 B9 103.8(2) . . ?
C1 B4 B8 104.2(2) . . ?
B9 B4 B8 60.57(17) . . ?
C1 B4 B7 58.17(15) . 2_556 ?
B9 B4 B7 59.71(16) . 2_556 ?
B8 B4 B7 108.2(2) . 2_556 ?
C1 B4 B3 59.65(15) . . ?
B9 B4 B3 108.8(2) . . ?
B8 B4 B3 59.67(16) . . ?
B7 B4 B3 109.1(2) 2_556 . ?
C1 B4 H4 125.4 . . ?
B9 B4 H4 122.4 . . ?
B8 B4 H4 122.5 . . ?
B7 B4 H4 121.3 2_556 . ?
B3 B4 H4 120.5 . . ?
C1 B7 B9 104.0(2) 2_556 2_556 ?
C1 B7 B8 104.5(2) 2_556 . ?
B9 B7 B8 60.70(17) 2_556 . ?
C1 B7 B4 58.42(15) 2_556 2_556 ?
B9 B7 B4 59.78(16) 2_556 2_556 ?
B8 B7 B4 108.6(2) . 2_556 ?
C1 B7 B3 59.93(15) 2_556 . ?
B9 B7 B3 109.0(2) 2_556 . ?
B8 B7 B3 59.70(16) . . ?
B4 B7 B3 109.7(2) 2_556 . ?
C1 B7 H7 125.1 2_556 . ?
B9 B7 H7 122.3 2_556 . ?
B8 B7 H7 122.3 . . ?
B4 B7 H7 121.0 2_556 . ?
B3 B7 H7 120.3 . . ?
B4 B8 B7 107.9(2) . . ?
B4 B8 B3 60.70(16) . . ?
B7 B8 B3 60.61(16) . . ?
B4 B8 B9 59.63(16) . . ?
B7 B8 B9 107.3(2) . . ?
B3 B8 B9 108.85(19) . . ?
B4 B8 B9 107.4(2) . 2_556 ?
B7 B8 B9 59.51(16) . 2_556 ?
B3 B8 B9 108.8(2) . 2_556 ?
B9 B8 B9 59.68(19) . 2_556 ?
B4 B8 H8 121.9 . . ?
B7 B8 H8 122.1 . . ?
B3 B8 H8 120.5 . . ?
B9 B8 H8 122.0 . . ?
B9 B8 H8 122.0 2_556 . ?
B7 B9 B4 60.51(16) 2_556 . ?
B7 B9 B9 107.78(19) 2_556 2_556 ?
B4 B9 B9 108.03(19) . 2_556 ?
B7 B9 B8 108.23(19) 2_556 . ?
B4 B9 B8 59.80(17) . . ?
B9 B9 B8 60.2(2) 2_556 . ?
B7 B9 B8 59.79(17) 2_556 2_556 ?
B4 B9 B8 108.45(19) . 2_556 ?
B9 B9 B8 60.1(2) 2_556 2_556 ?
B8 B9 B8 108.5(2) . 2_556 ?
B7 B9 H9 121.7 2_556 . ?
B4 B9 H9 121.5 . . ?
B9 B9 H9 121.8 2_556 . ?
B8 B9 H9 121.5 . . ?
B8 B9 H9 121.5 2_556 . ?
B3 C3 H3A 109.5 . . ?
B3 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
B3 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C1 1.613(5) 2_556 ?
C1 B7 1.694(4) 2_556 ?
C1 B4 1.698(4) . ?
C1 B3 1.738(4) . ?
C1 B3 1.742(4) 2_556 ?
C1 H1 1.1200 . ?
B3 C3 1.573(4) . ?
B3 C1 1.742(4) 2_556 ?
B3 B8 1.773(4) . ?
B3 B7 1.790(4) . ?
B3 B4 1.792(4) . ?
B4 B9 1.770(4) . ?
B4 B8 1.773(4) . ?
B4 B7 1.783(4) 2_556 ?
B4 H4 1.1200 . ?
B7 C1 1.694(3) 2_556 ?
B7 B9 1.768(4) 2_556 ?
B7 B8 1.773(4) . ?
B7 B4 1.783(4) 2_556 ?
B7 H7 1.1200 . ?
B8 B9 1.786(4) . ?
B8 B9 1.790(4) 2_556 ?
B8 H8 1.1200 . ?
B9 B7 1.768(4) 2_556 ?
B9 B9 1.779(6) 2_556 ?
B9 B8 1.790(4) 2_556 ?
B9 H9 1.1200 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
