#------------------------------------------------------------------------------
#$Date: 2019-11-23 11:39:10 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233126 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/85/4348579.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_4348579
loop_
_publ_author_name
'Burt, Jennifer'
'Emsley, James W.'
'Levason, William'
'Reid, Gillian'
'Tinkler, Iain S.'
_publ_section_title
;
 Systematics of BX3 and BX2(+) Complexes (X = F, Cl, Br, I) with Neutral
 Diphosphine and Diarsine Ligands.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8852
_journal_page_last               8864
_journal_paper_doi               10.1021/acs.inorgchem.6b01375
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C10 H16 B I2 P2, I3'
_chemical_formula_sum            'C10 H16 B I5 P2'
_chemical_formula_weight         843.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 97.751(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.702(2)
_cell_length_b                   17.454(3)
_cell_length_c                   12.615(2)
_cell_measurement_reflns_used    6103
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.8
_cell_volume                     2116.7(7)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18682
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.072
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           55.0
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    7.484
_exptl_absorpt_correction_T_max  0.807
_exptl_absorpt_correction_T_min  0.622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.647
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.968
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         4150
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0282
_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/[σ²(Fo²)+(0.0236P)²+8.6490P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0647
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3447
_reflns_number_total             4150
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b01375_si_011.cif
_cod_data_source_block           2015rwz1008b
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4348579
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
I1 I 0.03507(4) 0.19077(2) 0.48376(3) 0.02185(10) Uani 1 1 d . .
I2 I 0.04076(5) 0.39728(2) 0.41511(3) 0.02436(10) Uani 1 1 d . .
I3 I 0.50769(4) 0.10504(2) 0.61337(3) 0.02476(10) Uani 1 1 d . .
I4 I 0.45483(4) 0.05674(2) 0.82287(3) 0.02900(11) Uani 1 1 d . .
I5 I 0.57987(5) 0.16038(3) 0.40722(4) 0.03788(12) Uani 1 1 d . .
P1 P -0.11448(16) 0.33381(8) 0.62286(11) 0.0174(3) Uani 1 1 d . .
P2 P 0.19416(15) 0.32867(8) 0.65236(11) 0.0170(3) Uani 1 1 d . .
B1 B 0.0394(7) 0.3093(4) 0.5426(5) 0.0162(13) Uani 1 1 d . .
C1 C -0.2654(6) 0.3773(4) 0.5494(5) 0.0281(14) Uani 1 1 d . .
H1A H -0.3071 0.3419 0.4938 0.042 Uiso 1 1 calc R U
H1B H -0.2385 0.4247 0.5161 0.042 Uiso 1 1 calc R U
H1C H -0.3331 0.3889 0.5982 0.042 Uiso 1 1 calc R U
C2 C -0.1739(7) 0.2535(4) 0.6935(5) 0.0261(14) Uani 1 1 d . .
H2A H -0.0940 0.2280 0.7347 0.039 Uiso 1 1 calc R U
H2B H -0.2224 0.2172 0.6421 0.039 Uiso 1 1 calc R U
H2C H -0.2376 0.2715 0.7422 0.039 Uiso 1 1 calc R U
C3 C -0.0268(6) 0.4020(3) 0.7173(4) 0.0145(11) Uani 1 1 d . .
C4 C -0.0971(6) 0.4519(3) 0.7774(4) 0.0188(12) Uani 1 1 d . .
H4 H -0.1958 0.4520 0.7700 0.023 Uiso 1 1 calc R U
C5 C -0.0205(7) 0.5013(3) 0.8479(5) 0.0234(13) Uani 1 1 d . .
H5 H -0.0677 0.5358 0.8889 0.028 Uiso 1 1 calc R U
C6 C 0.1232(7) 0.5015(3) 0.8601(5) 0.0231(13) Uani 1 1 d . .
H6 H 0.1737 0.5360 0.9090 0.028 Uiso 1 1 calc R U
C7 C 0.1941(7) 0.4515(3) 0.8012(4) 0.0216(13) Uani 1 1 d . .
H7 H 0.2929 0.4513 0.8095 0.026 Uiso 1 1 calc R U
C8 C 0.1184(6) 0.4015(3) 0.7297(4) 0.0143(11) Uani 1 1 d . .
C9 C 0.3515(6) 0.3609(4) 0.6064(5) 0.0303(15) Uani 1 1 d . .
H9A H 0.4231 0.3693 0.6680 0.045 Uiso 1 1 calc R U
H9B H 0.3337 0.4090 0.5668 0.045 Uiso 1 1 calc R U
H9C H 0.3838 0.3220 0.5594 0.045 Uiso 1 1 calc R U
C10 C 0.2395(6) 0.2481(3) 0.7373(5) 0.0225(13) Uani 1 1 d . .
H10A H 0.2778 0.2075 0.6964 0.034 Uiso 1 1 calc R U
H10B H 0.1563 0.2291 0.7652 0.034 Uiso 1 1 calc R U
H10C H 0.3092 0.2636 0.7971 0.034 Uiso 1 1 calc R U
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
I4 I3 I5 175.77(2)
C1 P1 C2 107.0(3)
C1 P1 C3 109.9(3)
C2 P1 C3 109.8(3)
C1 P1 B1 116.8(3)
C2 P1 B1 113.8(3)
C3 P1 B1 99.2(3)
C10 P2 C9 106.8(3)
C10 P2 C8 108.3(3)
C9 P2 C8 112.2(3)
C10 P2 B1 113.4(3)
C9 P2 B1 115.9(3)
C8 P2 B1 100.1(3)
P2 B1 P1 99.4(3)
P2 B1 I1 112.6(3)
P1 B1 I1 113.5(3)
P2 B1 I2 108.5(3)
P1 B1 I2 107.6(3)
I1 B1 I2 114.1(3)
P1 C1 H1A 109.5
P1 C1 H1B 109.5
H1A C1 H1B 109.5
P1 C1 H1C 109.5
H1A C1 H1C 109.5
H1B C1 H1C 109.5
P1 C2 H2A 109.5
P1 C2 H2B 109.5
H2A C2 H2B 109.5
P1 C2 H2C 109.5
H2A C2 H2C 109.5
H2B C2 H2C 109.5
C4 C3 C8 120.2(5)
C4 C3 P1 123.3(4)
C8 C3 P1 116.5(4)
C5 C4 C3 118.8(6)
C5 C4 H4 120.6
C3 C4 H4 120.6
C4 C5 C6 121.4(5)
C4 C5 H5 119.3
C6 C5 H5 119.3
C5 C6 C7 120.3(6)
C5 C6 H6 119.9
C7 C6 H6 119.9
C6 C7 C8 119.0(6)
C6 C7 H7 120.5
C8 C7 H7 120.5
C7 C8 C3 120.4(5)
C7 C8 P2 124.8(4)
C3 C8 P2 114.8(4)
P2 C9 H9A 109.5
P2 C9 H9B 109.5
H9A C9 H9B 109.5
P2 C9 H9C 109.5
H9A C9 H9C 109.5
H9B C9 H9C 109.5
P2 C10 H10A 109.5
P2 C10 H10B 109.5
H10A C10 H10B 109.5
P2 C10 H10C 109.5
H10A C10 H10C 109.5
H10B C10 H10C 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
I1 B1 2.197(6)
I2 B1 2.224(6)
I3 I4 2.8851(7)
I3 I5 2.9459(7)
P1 C1 1.792(6)
P1 C2 1.797(6)
P1 C3 1.812(5)
P1 B1 1.961(6)
P2 C10 1.787(6)
P2 C9 1.795(6)
P2 C8 1.817(5)
P2 B1 1.930(7)
C1 H1A 0.9800
C1 H1B 0.9800
C1 H1C 0.9800
C2 H2A 0.9800
C2 H2B 0.9800
C2 H2C 0.9800
C3 C4 1.392(7)
C3 C8 1.397(8)
C4 C5 1.380(8)
C4 H4 0.9500
C5 C6 1.383(9)
C5 H5 0.9500
C6 C7 1.388(8)
C6 H6 0.9500
C7 C8 1.391(8)
C7 H7 0.9500
C9 H9A 0.9800
C9 H9B 0.9800
C9 H9C 0.9800
C10 H10A 0.9800
C10 H10B 0.9800
C10 H10C 0.9800
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C2 H2A I2 0.98 3.30 4.184(7) 151.5 4_566
C2 H2B I3 0.98 3.25 4.055(6) 140.5 1_455
C2 H2C I5 0.98 3.14 4.120(6) 174.7 4_466
C4 H4 I4 0.95 3.20 3.976(6) 140.3 2_556
C9 H9A I5 0.98 3.23 4.144(7) 155.4 4_566
C10 H10A I3 0.98 3.15 4.068(6) 157.4 .
C10 H10B I2 0.98 3.21 4.044(6) 144.6 4_566
C10 H10C I5 0.98 3.10 4.017(6) 156.6 4_566
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C1 P1 C3 C4 40.7(5)
C2 P1 C3 C4 -76.7(5)
B1 P1 C3 C4 163.7(5)
C1 P1 C3 C8 -140.5(4)
C2 P1 C3 C8 102.0(4)
B1 P1 C3 C8 -17.5(5)
C8 C3 C4 C5 0.8(8)
P1 C3 C4 C5 179.5(4)
C3 C4 C5 C6 -0.4(8)
C4 C5 C6 C7 -0.1(8)
C5 C6 C7 C8 0.2(8)
C6 C7 C8 C3 0.1(8)
C6 C7 C8 P2 -176.2(4)
C4 C3 C8 C7 -0.7(8)
P1 C3 C8 C7 -179.4(4)
C4 C3 C8 P2 176.0(4)
P1 C3 C8 P2 -2.8(5)
C10 P2 C8 C7 79.6(5)
C9 P2 C8 C7 -37.9(6)
B1 P2 C8 C7 -161.4(5)
C10 P2 C8 C3 -96.9(4)
C9 P2 C8 C3 145.6(4)
B1 P2 C8 C3 22.1(4)
