#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/65/2236522.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2236522
loop_
_publ_author_name
'Mayo, Dennis H.'
'Peng, Yang'
'Zavalij, Peter'
'Bowen, Kit H.'
'Eichhorn, Bryan W.'
_publ_section_title
;
 Tetrabromidobis(dicyclohexylphosphane-κP)digallium(Ga---Ga)
;
_journal_coeditor_code           NK2174
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1245
_journal_paper_doi               10.1107/S1600536812035982
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Ga2 Br4 (C12 H23 P)2]'
_chemical_formula_moiety         'C24 H46 Br4 Ga2 P2'
_chemical_formula_sum            'C24 H46 Br4 Ga2 P2'
_chemical_formula_weight         855.63
_chemical_name_systematic
;
Tetrabromidobis(dicyclohexylphosphane-κP)digallium
(Ga---Ga)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 & ZCIF'
_cell_angle_alpha                90.00
_cell_angle_beta                 109.177(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.6095(11)
_cell_length_b                   13.7083(16)
_cell_length_c                   13.3305(16)
_cell_measurement_reflns_used    12733
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      2.7
_cell_volume                     1658.6(3)
_computing_cell_refinement       'SAINT (Bruker, 2010)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_computing_molecular_graphics    'XSHELL (Bruker, 2010)'
_computing_publication_material  'APEX2 (Bruker, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX2 CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0149
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24854
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    6.551
_exptl_absorpt_correction_T_max  0.288
_exptl_absorpt_correction_T_min  0.185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.881
_refine_diff_density_min         -0.936
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         4842
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0340
_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)+(0.01P)²+4.865P], P=(max(Fo²,0)+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0680
_reflns_number_gt                4253
_reflns_number_total             4842
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            nk2174.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2236522
_cod_database_fobs_code          2236522
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Ga Ga1 0.43950(3) 0.06462(2) 0.53291(2) 0.02724(7) Uani d . 1 1 . .
Br Br1 0.58862(3) 0.20359(2) 0.60235(3) 0.04156(8) Uani d . 1 1 . .
Br Br2 0.33747(4) 0.01282(3) 0.66273(3) 0.04888(9) Uani d . 1 1 . .
P P1 0.23183(7) 0.14796(5) 0.40942(5) 0.02762(13) Uani d . 1 1 . .
H H1 0.274(4) 0.225(2) 0.368(3) 0.043(9) Uiso d . 1 1 . .
C C11 0.0946(13) 0.1955(10) 0.4656(12) 0.0339(18) Uani d PDU 0.620(13) 1 A 1
H H11 0.0698 0.1412 0.5069 0.041 Uiso calc PR 0.620(13) 1 A 1
C C12 -0.0495(10) 0.2268(7) 0.3805(7) 0.0453(18) Uani d PDU 0.620(13) 1 A 1
H H12A -0.0287 0.2777 0.3348 0.054 Uiso calc PR 0.620(13) 1 A 1
H H12B -0.0943 0.1702 0.3353 0.054 Uiso calc PR 0.620(13) 1 A 1
C C13 -0.1573(10) 0.2667(8) 0.4336(8) 0.066(2) Uani d PDU 0.620(13) 1 A 1
H H13A -0.2484 0.2890 0.3782 0.080 Uiso calc PR 0.620(13) 1 A 1
H H13B -0.1844 0.2139 0.4743 0.080 Uiso calc PR 0.620(13) 1 A 1
C C14 -0.0905(13) 0.3506(7) 0.5072(9) 0.071(3) Uani d PDU 0.620(13) 1 A 1
H H14A -0.0680 0.4049 0.4661 0.085 Uiso calc PR 0.620(13) 1 A 1
H H14B -0.1619 0.3745 0.5408 0.085 Uiso calc PR 0.620(13) 1 A 1
C C15 0.0478(13) 0.3180(11) 0.5913(9) 0.076(3) Uani d PDU 0.620(13) 1 A 1
H H15A 0.0234 0.2671 0.6355 0.092 Uiso calc PR 0.620(13) 1 A 1
H H15B 0.0918 0.3739 0.6380 0.092 Uiso calc PR 0.620(13) 1 A 1
C C16 0.1608(11) 0.2771(13) 0.5433(12) 0.0610(18) Uani d PDU 0.620(13) 1 A 1
H H16A 0.1945 0.3300 0.5063 0.073 Uiso calc PR 0.620(13) 1 A 1
H H16B 0.2475 0.2522 0.6009 0.073 Uiso calc PR 0.620(13) 1 A 1
C C11A 0.114(2) 0.2078(18) 0.475(2) 0.0339(18) Uani d PD 0.380(13) 1 A 2
H H11A 0.0753 0.1557 0.5109 0.041 Uiso calc PR 0.380(13) 1 A 2
C C12A -0.0197(17) 0.2566(12) 0.3935(12) 0.0453(18) Uani d PD 0.380(13) 1 A 2
H H12C 0.0143 0.3053 0.3518 0.054 Uiso calc PR 0.380(13) 1 A 2
H H12D -0.0788 0.2068 0.3438 0.054 Uiso calc PR 0.380(13) 1 A 2
C C13A -0.1153(15) 0.3069(13) 0.4503(13) 0.066(2) Uani d PD 0.380(13) 1 A 2
H H13C -0.1967 0.3420 0.3972 0.080 Uiso calc PR 0.380(13) 1 A 2
H H13D -0.1595 0.2568 0.4839 0.080 Uiso calc PR 0.380(13) 1 A 2
C C14A -0.030(2) 0.3779(12) 0.5336(14) 0.071(3) Uani d PD 0.380(13) 1 A 2
H H14C 0.0048 0.4325 0.4992 0.085 Uiso calc PR 0.380(13) 1 A 2
H H14D -0.0945 0.4051 0.5710 0.085 Uiso calc PR 0.380(13) 1 A 2
C C15A 0.100(2) 0.3296(19) 0.6123(14) 0.076(3) Uani d PD 0.380(13) 1 A 2
H H15C 0.0645 0.2810 0.6532 0.092 Uiso calc PR 0.380(13) 1 A 2
H H15D 0.1580 0.3792 0.6628 0.092 Uiso calc PR 0.380(13) 1 A 2
C C16A 0.2001(18) 0.279(2) 0.560(2) 0.0610(18) Uani d PD 0.380(13) 1 A 2
H H16C 0.2474 0.3281 0.5276 0.073 Uiso calc PR 0.380(13) 1 A 2
H H16D 0.2787 0.2429 0.6143 0.073 Uiso calc PR 0.380(13) 1 A 2
C C21 0.1299(3) 0.0773(2) 0.2924(2) 0.0305(5) Uani d . 1 1 A .
H H21 0.0502 0.1198 0.2458 0.037 Uiso calc R 1 1 . .
C C22 0.0573(3) -0.0116(2) 0.3232(3) 0.0414(7) Uani d . 1 1 . .
H H22A 0.1338 -0.0552 0.3695 0.050 Uiso calc R 1 1 A .
H H22B -0.0080 0.0095 0.3631 0.050 Uiso calc R 1 1 . .
C C23 -0.0321(4) -0.0665(3) 0.2234(3) 0.0564(9) Uani d . 1 1 A .
H H23A -0.0759 -0.1255 0.2437 0.068 Uiso calc R 1 1 . .
H H23B -0.1135 -0.0245 0.1801 0.068 Uiso calc R 1 1 . .
C C24 0.0637(4) -0.0955(3) 0.1588(3) 0.0574(10) Uani d . 1 1 . .
H H24A 0.0021 -0.1279 0.0928 0.069 Uiso calc R 1 1 A .
H H24B 0.1382 -0.1431 0.1997 0.069 Uiso calc R 1 1 . .
C C25 0.1420(4) -0.0083(3) 0.1301(3) 0.0539(9) Uani d . 1 1 A .
H H25A 0.0682 0.0356 0.0818 0.065 Uiso calc R 1 1 . .
H H25B 0.2088 -0.0315 0.0922 0.065 Uiso calc R 1 1 . .
C C26 0.2313(3) 0.0484(2) 0.2299(2) 0.0384(6) Uani d . 1 1 . .
H H26A 0.3128 0.0073 0.2746 0.046 Uiso calc R 1 1 A .
H H26B 0.2744 0.1076 0.2093 0.046 Uiso calc R 1 1 . .
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Br2 Ga1 Br1 . 107.306(18) yes
Br2 Ga1 P1 . 101.11(2) yes
Br1 Ga1 P1 . 98.25(2) yes
Br2 Ga1 Ga1 3_656 114.05(2) yes
Br1 Ga1 Ga1 3_656 115.13(2) yes
P1 Ga1 Ga1 3_656 118.93(2) yes
C21 P1 C11 . 106.3(4) ?
C21 P1 Ga1 . 115.00(9) ?
C11 P1 Ga1 . 115.7(4) ?
C21 P1 H1 . 102.5(15) ?
C11 P1 H1 . 104.4(16) ?
Ga1 P1 H1 . 111.6(15) ?
C16 C11 C12 . 111.9(5) ?
C16 C11 P1 . 110.1(8) ?
C12 C11 P1 . 113.1(8) ?
C16 C11 H11 . 107.1 ?
C12 C11 H11 . 107.1 ?
P1 C11 H11 . 107.1 ?
C13 C12 C11 . 110.0(6) ?
C13 C12 H12A . 109.7 ?
C11 C12 H12A . 109.7 ?
C13 C12 H12B . 109.7 ?
C11 C12 H12B . 109.7 ?
H12A C12 H12B . 108.2 ?
C14 C13 C12 . 111.3(6) ?
C14 C13 H13A . 109.4 ?
C12 C13 H13A . 109.4 ?
C14 C13 H13B . 109.4 ?
C12 C13 H13B . 109.4 ?
H13A C13 H13B . 108.0 ?
C15 C14 C13 . 110.0(6) ?
C15 C14 H14A . 109.7 ?
C13 C14 H14A . 109.7 ?
C15 C14 H14B . 109.7 ?
C13 C14 H14B . 109.7 ?
H14A C14 H14B . 108.2 ?
C14 C15 C16 . 111.8(6) ?
C14 C15 H15A . 109.2 ?
C16 C15 H15A . 109.2 ?
C14 C15 H15B . 109.2 ?
C16 C15 H15B . 109.2 ?
H15A C15 H15B . 107.9 ?
C11 C16 C15 . 111.0(7) ?
C11 C16 H16A . 109.4 ?
C15 C16 H16A . 109.4 ?
C11 C16 H16B . 109.4 ?
C15 C16 H16B . 109.4 ?
H16A C16 H16B . 108.0 ?
C22 C21 C26 . 111.7(3) ?
C22 C21 P1 . 111.0(2) ?
C26 C21 P1 . 110.16(19) ?
C22 C21 H21 . 107.9 ?
C26 C21 H21 . 107.9 ?
P1 C21 H21 . 107.9 ?
C23 C22 C21 . 109.6(3) ?
C23 C22 H22A . 109.7 ?
C21 C22 H22A . 109.7 ?
C23 C22 H22B . 109.7 ?
C21 C22 H22B . 109.7 ?
H22A C22 H22B . 108.2 ?
C24 C23 C22 . 110.7(3) ?
C24 C23 H23A . 109.5 ?
C22 C23 H23A . 109.5 ?
C24 C23 H23B . 109.5 ?
C22 C23 H23B . 109.5 ?
H23A C23 H23B . 108.1 ?
C23 C24 C25 . 112.4(3) ?
C23 C24 H24A . 109.1 ?
C25 C24 H24A . 109.1 ?
C23 C24 H24B . 109.1 ?
C25 C24 H24B . 109.1 ?
H24A C24 H24B . 107.9 ?
C24 C25 C26 . 111.1(3) ?
C24 C25 H25A . 109.4 ?
C26 C25 H25A . 109.4 ?
C24 C25 H25B . 109.4 ?
C26 C25 H25B . 109.4 ?
H25A C25 H25B . 108.0 ?
C21 C26 C25 . 109.2(3) ?
C21 C26 H26A . 109.8 ?
C25 C26 H26A . 109.8 ?
C21 C26 H26B . 109.8 ?
C25 C26 H26B . 109.8 ?
H26A C26 H26B . 108.3 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ga1 Br2 . 2.3612(5) yes
Ga1 Br1 . 2.3807(5) yes
Ga1 P1 . 2.4164(7) yes
Ga1 Ga1 3_656 2.4353(6) yes
P1 C21 . 1.824(3) ?
P1 C11A . 1.83(2) ?
P1 C11 . 1.837(13) ?
P1 H1 . 1.31(3) ?
C11 C16 . 1.516(7) ?
C11 C12 . 1.535(6) ?
C11 H11 . 1.0000 ?
C12 C13 . 1.534(7) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C13 C14 . 1.512(10) ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
C14 C15 . 1.499(9) ?
C14 H14A . 0.9900 ?
C14 H14B . 0.9900 ?
C15 C16 . 1.536(7) ?
C15 H15A . 0.9900 ?
C15 H15B . 0.9900 ?
C16 H16A . 0.9900 ?
C16 H16B . 0.9900 ?
C21 C22 . 1.526(4) ?
C21 C26 . 1.527(4) ?
C21 H21 . 1.0000 ?
C22 C23 . 1.523(5) ?
C22 H22A . 0.9900 ?
C22 H22B . 0.9900 ?
C23 C24 . 1.506(6) ?
C23 H23A . 0.9900 ?
C23 H23B . 0.9900 ?
C24 C25 . 1.527(6) ?
C24 H24A . 0.9900 ?
C24 H24B . 0.9900 ?
C25 C26 . 1.537(4) ?
C25 H25A . 0.9900 ?
C25 H25B . 0.9900 ?
C26 H26A . 0.9900 ?
C26 H26B . 0.9900 ?
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_site_symmetry_1
_geom_torsion
Br2 Ga1 P1 C21 . -99.72(10)
Br1 Ga1 P1 C21 . 150.72(10)
Ga1 Ga1 P1 C21 3_656 25.94(11)
Br2 Ga1 P1 C11 . 24.9(6)
Br1 Ga1 P1 C11 . -84.6(6)
Ga1 Ga1 P1 C11 3_656 150.6(6)
C21 P1 C11 C16 . -164.2(8)
Ga1 P1 C11 C16 . 66.8(9)
C21 P1 C11 C12 . -38.2(11)
Ga1 P1 C11 C12 . -167.2(7)
C16 C11 C12 C13 . -54.2(12)
P1 C11 C12 C13 . -179.3(8)
C11 C12 C13 C14 . 56.9(10)
C12 C13 C14 C15 . -58.8(10)
C13 C14 C15 C16 . 57.5(12)
C12 C11 C16 C15 . 53.3(13)
P1 C11 C16 C15 . -180.0(11)
C14 C15 C16 C11 . -55.2(13)
C11 P1 C21 C22 . -64.9(6)
Ga1 P1 C21 C22 . 64.5(2)
C11A P1 C21 C26 . 167.9(11)
C11 P1 C21 C26 . 170.9(6)
Ga1 P1 C21 C26 . -59.8(2)
C26 C21 C22 C23 . -59.0(3)
P1 C21 C22 C23 . 177.6(2)
C21 C22 C23 C24 . 56.9(4)
C22 C23 C24 C25 . -55.9(4)
C23 C24 C25 C26 . 55.1(4)
C22 C21 C26 C25 . 57.8(3)
P1 C21 C26 C25 . -178.3(2)
C24 C25 C26 C21 . -54.8(4)
