# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gecl2diphos8
_audit_creation_date             2012-11-27
_audit_creation_method           
;
  Olex2 1.2
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
# start Validation Reply Form
_vrf_PLAT029_gecl2diphos8        
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.652       
RESPONSE: Data are collected using a diamond anvil cell which has a limited 
opening angle which restricts the data accessible to measure.
This typically resulta in very low completeness although in this
case the wavelength of 0.48 angstrom improves completeness.
;

_chemical_name_common            ?
_chemical_name_systematic        
;
'Dichlorido(1,2-bis(dimethylphosphino)benzene)germanium(II)'
;
_chemical_formula_moiety         'C10 H16 Cl2 Ge P2'
_chemical_formula_sum            'C10 H16 Cl2 Ge P2'
_chemical_formula_weight         341.66
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0007 0.0007 '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'
Cl Cl 0.0777 0.0747 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.3342 0.9482 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0517 0.0444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z-1/2'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   26.73(4)
_cell_length_b                   6.863(8)
_cell_length_c                   13.068(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.22(7)
_cell_angle_gamma                90.00
_cell_volume                     2250(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       4800000 # kpascals = 48kbar
_cell_measurement_reflns_used    702
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      18.4
_exptl_absorpt_coefficient_mu    1.207
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.018
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ?
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.1337
_diffrn_reflns_av_unetI/netI     0.1364
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7078
_diffrn_reflns_theta_full        18.47
_diffrn_reflns_theta_max         18.47
_diffrn_reflns_theta_min         2.10
_diffrn_ambient_temperature      293(2)
_diffrn_source_type              'DLS beamline I19'
_diffrn_source                   synchrotron
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'
_diffrn_radiation_type           Synchrotron
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_ambient_pressure         4800000 #kpascals = 48kbar
_diffrn_measurement_specimen_support 'Diamond Anvil Cell'

_diffrn_measured_fraction_theta_full 0.652
_diffrn_measured_fraction_theta_max 0.652
_diffrn_radiation_wavelength     0.48590
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                1238
_reflns_number_total             1697
_reflns_threshold_expression     >2σ(I)
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2011)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2011)
;
_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  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.818
_refine_diff_density_min         -0.844
_refine_diff_density_rms         0.209
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         1697
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1416
_refine_ls_R_factor_gt           0.0938
_refine_ls_restrained_S_all      1.126
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+82.2205P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1526
_refine_ls_wR_factor_ref         0.1784
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  H4 of C4, H5 of C5, H6 of C6, H7 of C7
 At 1.5 times of:
  {H9A,H9B,H9C} of C9, {H10A,H10B,H10C} of C10, {H2A,H2B,H2C} of C2, {H1A,H1B,
  H1C} of C1
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7)
2.b Fitted hexagon refined as free rotating group:
 C3(C4,C5,C6,C7,C8)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.55365(7) 0.61619(14) 0.72290(10) 0.0185(5) Uani 1 1 d . . .
Cl1 Cl 0.48123(16) 0.8109(4) 0.5901(2) 0.0230(11) Uani 1 1 d . . .
Cl2 Cl 0.64905(15) 0.5038(3) 0.8384(2) 0.0207(9) Uani 1 1 d . . .
P1 P 0.59725(16) 0.5995(3) 0.5875(2) 0.0148(10) Uani 1 1 d . . .
P2 P 0.60247(16) 0.9147(3) 0.7619(2) 0.0143(10) Uani 1 1 d . . .
C1 C 0.6309(6) 0.3777(13) 0.5782(9) 0.017(2) Uiso 1 1 d . . .
H1A H 0.6599 0.3561 0.6454 0.026 Uiso 1 1 calc R . .
H1B H 0.6446 0.3874 0.5195 0.026 Uiso 1 1 calc R . .
H1C H 0.6063 0.2707 0.5649 0.026 Uiso 1 1 calc R . .
C2 C 0.5558(6) 0.6748(13) 0.4543(9) 0.019(2) Uiso 1 1 d . . .
H2A H 0.5240 0.5969 0.4307 0.028 Uiso 1 1 calc R . .
H2B H 0.5748 0.6584 0.4044 0.028 Uiso 1 1 calc R . .
H2C H 0.5464 0.8094 0.4561 0.028 Uiso 1 1 calc R . .
C3 C 0.6526(3) 0.7660(9) 0.6280(6) 0.018(2) Uiso 1 1 d G . .
C4 C 0.6923(3) 0.7562(8) 0.5819(5) 0.018(2) Uiso 1 1 d G . .
H4 H 0.6913 0.6589 0.5317 0.022 Uiso 1 1 calc R . .
C5 C 0.7334(3) 0.8920(10) 0.6108(6) 0.027(2) Uiso 1 1 d G . .
H5 H 0.7599 0.8855 0.5800 0.032 Uiso 1 1 calc R . .
C6 C 0.7349(3) 1.0374(9) 0.6858(6) 0.026(2) Uiso 1 1 d G . .
H6 H 0.7624 1.1282 0.7052 0.031 Uiso 1 1 calc R . .
C7 C 0.6952(3) 1.0471(8) 0.7319(5) 0.019(2) Uiso 1 1 d G . .
H7 H 0.6962 1.1445 0.7821 0.023 Uiso 1 1 calc R . .
C8 C 0.6541(3) 0.9114(9) 0.7030(6) 0.016(2) Uiso 1 1 d G . .
C9 C 0.5636(6) 1.1268(13) 0.7122(10) 0.019(2) Uiso 1 1 d . . .
H9A H 0.5449 1.1137 0.6353 0.029 Uiso 1 1 calc R . .
H9B H 0.5865 1.2386 0.7256 0.029 Uiso 1 1 calc R . .
H9C H 0.5384 1.1426 0.7490 0.029 Uiso 1 1 calc R . .
C10 C 0.6394(6) 0.9719(14) 0.9020(9) 0.021(2) Uiso 1 1 d . . .
H10A H 0.6521 1.1036 0.9071 0.031 Uiso 1 1 calc R . .
H10B H 0.6692 0.8847 0.9291 0.031 Uiso 1 1 calc R . .
H10C H 0.6167 0.9580 0.9445 0.031 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ge1 0.0215(15) 0.0148(6) 0.0202(7) -0.0001(4) 0.0084(9) -0.0014(5)
Cl1 0.020(4) 0.0220(14) 0.0263(18) 0.0025(10) 0.007(2) 0.0005(11)
Cl2 0.017(3) 0.0227(13) 0.0218(16) 0.0033(10) 0.006(2) 0.0029(11)
P1 0.014(3) 0.0162(13) 0.0134(16) -0.0018(9) 0.004(2) -0.0015(11)
P2 0.014(3) 0.0136(13) 0.0153(16) -0.0008(9) 0.005(2) 0.0008(10)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
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
Ge1 Cl1 2.494(5) . ?
Ge1 Cl2 2.592(5) . ?
Ge1 P1 2.435(4) . ?
Ge1 P2 2.387(4) . ?
P1 C1 1.794(11) . ?
P1 C2 1.786(13) . ?
P1 C3 1.798(7) . ?
P2 C8 1.798(6) . ?
P2 C9 1.775(12) . ?
P2 C10 1.797(13) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.3900 . ?
C3 C8 1.3900 . ?
C4 H4 0.9300 . ?
C4 C5 1.3900 . ?
C5 H5 0.9300 . ?
C5 C6 1.3900 . ?
C6 H6 0.9300 . ?
C6 C7 1.3900 . ?
C7 H7 0.9300 . ?
C7 C8 1.3900 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?

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
Cl1 Ge1 Cl2 159.32(11) . . ?
P1 Ge1 Cl1 88.33(15) . . ?
P1 Ge1 Cl2 77.74(16) . . ?
P2 Ge1 Cl1 85.67(15) . . ?
P2 Ge1 Cl2 77.05(14) . . ?
P2 Ge1 P1 80.33(11) . . ?
C1 P1 Ge1 117.8(3) . . ?
C1 P1 C3 100.3(6) . . ?
C2 P1 Ge1 113.8(4) . . ?
C2 P1 C1 109.6(5) . . ?
C2 P1 C3 105.8(5) . . ?
C3 P1 Ge1 107.9(2) . . ?
C8 P2 Ge1 110.0(2) . . ?
C9 P2 Ge1 114.7(5) . . ?
C9 P2 C8 107.0(4) . . ?
C9 P2 C10 103.8(6) . . ?
C10 P2 Ge1 118.2(3) . . ?
C10 P2 C8 101.9(6) . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 P1 121.0(4) . . ?
C4 C3 C8 120.0 . . ?
C8 C3 P1 118.9(4) . . ?
C3 C4 H4 120.0 . . ?
C3 C4 C5 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 H6 120.0 . . ?
C5 C6 C7 120.0 . . ?
C7 C6 H6 120.0 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 C6 120.0 . . ?
C8 C7 H7 120.0 . . ?
C3 C8 P2 118.2(4) . . ?
C7 C8 P2 121.8(4) . . ?
C7 C8 C3 120.0 . . ?
P2 C9 H9A 109.5 . . ?
P2 C9 H9B 109.5 . . ?
P2 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P2 C10 H10A 109.5 . . ?
P2 C10 H10B 109.5 . . ?
P2 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ge1 P1 C3 C4 164.8(3) . . . . ?
Ge1 P1 C3 C8 -18.1(5) . . . . ?
Ge1 P2 C8 C3 12.7(5) . . . . ?
Ge1 P2 C8 C7 -166.2(4) . . . . ?
Cl1 Ge1 P1 C1 -143.2(6) . . . . ?
Cl1 Ge1 P1 C2 -12.8(4) . . . . ?
Cl1 Ge1 P1 C3 104.3(3) . . . . ?
Cl1 Ge1 P2 C8 -106.1(3) . . . . ?
Cl1 Ge1 P2 C9 14.5(4) . . . . ?
Cl1 Ge1 P2 C10 137.5(5) . . . . ?
Cl2 Ge1 P1 C1 52.2(6) . . . . ?
Cl2 Ge1 P1 C2 -177.4(4) . . . . ?
Cl2 Ge1 P1 C3 -60.3(3) . . . . ?
Cl2 Ge1 P2 C8 62.4(3) . . . . ?
Cl2 Ge1 P2 C9 -177.0(4) . . . . ?
Cl2 Ge1 P2 C10 -53.9(5) . . . . ?
P1 Ge1 P2 C8 -17.1(3) . . . . ?
P1 Ge1 P2 C9 103.5(4) . . . . ?
P1 Ge1 P2 C10 -133.4(5) . . . . ?
P1 C3 C4 C5 177.1(6) . . . . ?
P1 C3 C8 P2 4.0(5) . . . . ?
P1 C3 C8 C7 -177.1(6) . . . . ?
P2 Ge1 P1 C1 130.9(6) . . . . ?
P2 Ge1 P1 C2 -98.7(4) . . . . ?
P2 Ge1 P1 C3 18.4(3) . . . . ?
C1 P1 C3 C4 40.9(6) . . . . ?
C1 P1 C3 C8 -142.0(5) . . . . ?
C2 P1 C3 C4 -73.0(6) . . . . ?
C2 P1 C3 C8 104.1(5) . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C4 C3 C8 P2 -178.9(6) . . . . ?
C4 C3 C8 C7 0.0 . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C5 C6 C7 C8 0.0 . . . . ?
C6 C7 C8 P2 178.9(6) . . . . ?
C6 C7 C8 C3 0.0 . . . . ?
C8 C3 C4 C5 0.0 . . . . ?
C9 P2 C8 C3 -112.5(6) . . . . ?
C9 P2 C8 C7 68.6(7) . . . . ?
C10 P2 C8 C3 138.8(5) . . . . ?
C10 P2 C8 C7 -40.0(6) . . . . ?

_database_code_depnum_ccdc_archive 'CCDC 977894'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gecl2diphos1
_audit_creation_date             2012-11-23
_audit_creation_method           
;
  Olex2 1.2
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
# start Validation Reply Form
_vrf_PLAT029_gecl2diphos1        
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.449       
RESPONSE: Data are collected using a diamond anvil cell which has a limited 
opening angle which restricts the data accessible to measure.
This typically resulta in very low completeness although in this
case the wavelength of 0.48 angstrom improves completeness.
;


_chemical_name_common            ?
_chemical_name_systematic        
;
'Dichlorido(1,2-bis(dimethylphosphino)benzene)germanium(II)'
;
_chemical_formula_moiety         'C10 H16 Cl2 Ge P2'
_chemical_formula_sum            'C10 H16 Cl2 Ge P2'
_chemical_formula_weight         341.66
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0007 0.0007 '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'
Cl Cl 0.0777 0.0747 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.3342 0.9482 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0517 0.0444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z-1/2'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   27.82(8)
_cell_length_b                   7.38(2)
_cell_length_c                   13.96(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.73(16)
_cell_angle_gamma                90.00
_cell_volume                     2698(13)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    811
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       100000 # kpascals = 1kbar
_cell_measurement_theta_max      18.5
_cell_measurement_theta_min      2.0
_exptl_absorpt_coefficient_mu    1.007
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.2128
_diffrn_reflns_av_unetI/netI     0.1656
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7326
_diffrn_reflns_theta_full        16.86
_diffrn_reflns_theta_max         16.86
_diffrn_reflns_theta_min         1.96
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_pressure         100000 #kpascals = 1kbar
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.449
_diffrn_measured_fraction_theta_max 0.449
_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.48590
_diffrn_source                   synchrotron
_diffrn_source_type              'DLS beamline I19'
_diffrn_measurement_specimen_support 'Diamond Anvil Cell'

_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                726
_reflns_number_total             1078
_reflns_threshold_expression     >2σ(I)
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2011)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2011)
;
_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  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.168
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         1078
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1696
_refine_ls_R_factor_gt           0.0980
_refine_ls_restrained_S_all      1.096
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0854P)²+125.4731P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2153
_refine_ls_wR_factor_ref         0.2795
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  H7 of C7, H6 of C6, H4 of C4, H5 of C5
 At 1.5 times of:
  {H10A,H10B,H10C} of C10, {H1A,H1B,H1C} of C1, {H9A,H9B,H9C} of C9, {H2A,H2B,
  H2C} of C2
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7)
2.b Fitted hexagon refined as free rotating group:
 C3(C4,C5,C6,C7,C8)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.5572(2) 0.6202(2) 0.71825(19) 0.065(3) Uani 1 1 d . . .
Cl1 Cl 0.4862(5) 0.7937(7) 0.5994(5) 0.073(7) Uani 1 1 d . . .
Cl2 Cl 0.6486(5) 0.4929(6) 0.8320(5) 0.040(6) Uani 1 1 d . . .
P1 P 0.5976(4) 0.6194(6) 0.5914(4) 0.026(5) Uani 1 1 d . . .
P2 P 0.6035(5) 0.8964(5) 0.7601(5) 0.050(6) Uani 1 1 d . . .
C1 C 0.6312(16) 0.410(2) 0.5813(18) 0.033(4) Uiso 1 1 d . . .
H1A H 0.6567 0.3834 0.6459 0.050 Uiso 1 1 calc R . .
H1B H 0.6473 0.4252 0.5309 0.050 Uiso 1 1 calc R . .
H1C H 0.6072 0.3118 0.5619 0.050 Uiso 1 1 calc R . .
C2 C 0.564(2) 0.680(3) 0.4690(18) 0.047(5) Uiso 1 1 d . . .
H2A H 0.5351 0.6026 0.4425 0.070 Uiso 1 1 calc R . .
H2B H 0.5859 0.6666 0.4282 0.070 Uiso 1 1 calc R . .
H2C H 0.5536 0.8034 0.4672 0.070 Uiso 1 1 calc R . .
C3 C 0.6464(8) 0.7756(15) 0.6270(10) 0.033(4) Uiso 1 1 d G . .
C4 C 0.6850(9) 0.7715(15) 0.5846(10) 0.042(5) Uiso 1 1 d G . .
H4 H 0.6838 0.6870 0.5344 0.050 Uiso 1 1 calc R . .
C5 C 0.7253(8) 0.8935(18) 0.6172(12) 0.049(6) Uiso 1 1 d G . .
H5 H 0.7511 0.8908 0.5888 0.058 Uiso 1 1 calc R . .
C6 C 0.7270(8) 1.0198(17) 0.6922(11) 0.054(6) Uiso 1 1 d G . .
H6 H 0.7540 1.1014 0.7140 0.065 Uiso 1 1 calc R . .
C7 C 0.6885(9) 1.0239(16) 0.7346(10) 0.061(7) Uiso 1 1 d G . .
H7 H 0.6896 1.1083 0.7848 0.073 Uiso 1 1 calc R . .
C8 C 0.6482(8) 0.9018(16) 0.7021(11) 0.036(5) Uiso 1 1 d G . .
C9 C 0.5672(19) 1.099(2) 0.7169(19) 0.043(5) Uiso 1 1 d . . .
H9A H 0.5551 1.1024 0.6439 0.064 Uiso 1 1 calc R . .
H9B H 0.5884 1.2028 0.7431 0.064 Uiso 1 1 calc R . .
H9C H 0.5386 1.1009 0.7407 0.064 Uiso 1 1 calc R . .
C10 C 0.631(2) 0.925(3) 0.8912(19) 0.049(6) Uiso 1 1 d . . .
H10A H 0.6095 0.9976 0.9159 0.073 Uiso 1 1 calc R . .
H10B H 0.6639 0.9838 0.9059 0.073 Uiso 1 1 calc R . .
H10C H 0.6362 0.8084 0.9239 0.073 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ge1 0.135(8) 0.0273(10) 0.0465(17) -0.0017(9) 0.047(4) -0.0049(15)
Cl1 0.12(2) 0.042(3) 0.064(5) -0.001(3) 0.034(10) -0.002(4)
Cl2 0.028(19) 0.049(3) 0.038(4) 0.000(2) 0.004(8) -0.003(4)
P1 0.020(17) 0.033(2) 0.027(3) -0.0032(19) 0.010(7) -0.006(3)
P2 0.09(2) 0.027(2) 0.041(4) -0.005(2) 0.035(8) -0.003(4)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
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
Ge1 Cl1 2.465(13) . ?
Ge1 Cl2 2.672(14) . ?
Ge1 P1 2.395(9) . ?
Ge1 P2 2.376(9) . ?
P1 C1 1.84(3) . ?
P1 C2 1.70(3) . ?
P1 C3 1.723(18) . ?
P2 C8 1.697(17) . ?
P2 C9 1.79(3) . ?
P2 C10 1.74(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.3900 . ?
C3 C8 1.3900 . ?
C4 H4 0.9300 . ?
C4 C5 1.3900 . ?
C5 H5 0.9300 . ?
C5 C6 1.3900 . ?
C6 H6 0.9300 . ?
C6 C7 1.3900 . ?
C7 H7 0.9300 . ?
C7 C8 1.3900 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?

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
Cl1 Ge1 Cl2 165.4(3) . . ?
P1 Ge1 Cl1 88.4(4) . . ?
P1 Ge1 Cl2 81.3(4) . . ?
P2 Ge1 Cl1 88.0(4) . . ?
P2 Ge1 Cl2 80.1(4) . . ?
P2 Ge1 P1 80.4(3) . . ?
C1 P1 Ge1 115.9(6) . . ?
C2 P1 Ge1 120.7(15) . . ?
C2 P1 C1 105.0(12) . . ?
C2 P1 C3 102.8(14) . . ?
C3 P1 Ge1 107.8(5) . . ?
C3 P1 C1 102.3(14) . . ?
C8 P2 Ge1 109.1(5) . . ?
C8 P2 C9 103.9(12) . . ?
C8 P2 C10 111.1(19) . . ?
C9 P2 Ge1 115.9(15) . . ?
C10 P2 Ge1 111.9(10) . . ?
C10 P2 C9 104.7(12) . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.4 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 P1 120.6(8) . . ?
C4 C3 C8 120.0 . . ?
C8 C3 P1 119.3(8) . . ?
C3 C4 H4 120.0 . . ?
C3 C4 C5 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 H6 120.0 . . ?
C5 C6 C7 120.0 . . ?
C7 C6 H6 120.0 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 C6 120.0 . . ?
C8 C7 H7 120.0 . . ?
C3 C8 P2 119.9(8) . . ?
C7 C8 P2 119.9(9) . . ?
C7 C8 C3 120.0 . . ?
P2 C9 H9A 109.5 . . ?
P2 C9 H9B 109.5 . . ?
P2 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P2 C10 H10A 109.5 . . ?
P2 C10 H10B 109.5 . . ?
P2 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ge1 P1 C3 C4 162.4(7) . . . . ?
Ge1 P1 C3 C8 -14.9(10) . . . . ?
Ge1 P2 C8 C3 12.2(11) . . . . ?
Ge1 P2 C8 C7 -163.2(7) . . . . ?
Cl1 Ge1 P1 C1 -142.2(14) . . . . ?
Cl1 Ge1 P1 C2 -13.5(10) . . . . ?
Cl1 Ge1 P1 C3 104.0(7) . . . . ?
Cl1 Ge1 P2 C8 -103.9(8) . . . . ?
Cl1 Ge1 P2 C9 12.8(8) . . . . ?
Cl1 Ge1 P2 C10 132.8(17) . . . . ?
Cl2 Ge1 P1 C1 48.3(14) . . . . ?
Cl2 Ge1 P1 C2 176.9(10) . . . . ?
Cl2 Ge1 P1 C3 -65.5(7) . . . . ?
Cl2 Ge1 P2 C8 67.6(8) . . . . ?
Cl2 Ge1 P2 C9 -175.7(8) . . . . ?
Cl2 Ge1 P2 C10 -55.7(17) . . . . ?
P1 Ge1 P2 C8 -15.1(8) . . . . ?
P1 Ge1 P2 C9 101.6(8) . . . . ?
P1 Ge1 P2 C10 -138.5(17) . . . . ?
P1 C3 C4 C5 -177.3(11) . . . . ?
P1 C3 C8 P2 2.0(12) . . . . ?
P1 C3 C8 C7 177.3(11) . . . . ?
P2 Ge1 P1 C1 129.6(15) . . . . ?
P2 Ge1 P1 C2 -101.8(11) . . . . ?
P2 Ge1 P1 C3 15.8(7) . . . . ?
C1 P1 C3 C4 39.8(11) . . . . ?
C1 P1 C3 C8 -137.5(10) . . . . ?
C2 P1 C3 C4 -69.0(14) . . . . ?
C2 P1 C3 C8 113.7(13) . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C4 C3 C8 P2 -175.4(12) . . . . ?
C4 C3 C8 C7 0.0 . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C5 C6 C7 C8 0.0 . . . . ?
C6 C7 C8 P2 175.4(11) . . . . ?
C6 C7 C8 C3 0.0 . . . . ?
C8 C3 C4 C5 0.0 . . . . ?
C9 P2 C8 C3 -111.9(14) . . . . ?
C9 P2 C8 C7 72.7(14) . . . . ?
C10 P2 C8 C3 136.0(10) . . . . ?
C10 P2 C8 C7 -39.3(11) . . . . ?

_database_code_depnum_ccdc_archive 'CCDC 977895'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gecl2diphos6
_audit_creation_date             2012-11-26
_audit_creation_method           
;
  Olex2 1.2
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
# start Validation Reply Form
_vrf_PLAT029_gecl2diphos6        
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.656       
RESPONSE: Data are collected using a diamond anvil cell which has a limited 
opening angle which restricts the data accessible to measure.
This typically resulta in very low completeness although in this
case the wavelength of 0.48 angstrom improves completeness.
;

_chemical_name_common            ?
_chemical_name_systematic        
;
'Dichlorido(1,2-bis(dimethylphosphino)benzene)germanium(II)'
;
_chemical_formula_moiety         'C10 H16 Cl2 Ge P2'
_chemical_formula_sum            'C10 H16 Cl2 Ge P2'
_chemical_formula_weight         341.66
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0007 0.0007 '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'
Cl Cl 0.0777 0.0747 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.3342 0.9482 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0517 0.0444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z-1/2'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   27.99(4)
_cell_length_b                   7.325(10)
_cell_length_c                   13.88(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.29(8)
_cell_angle_gamma                90.00
_cell_volume                     2669(7)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    845
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      18.5
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       1100000 # kpascals = 11kbar
_exptl_absorpt_coefficient_mu    1.017
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.1417
_diffrn_reflns_av_unetI/netI     0.1431
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8543
_diffrn_reflns_theta_full        18.53
_diffrn_reflns_theta_max         18.53
_diffrn_reflns_theta_min         1.97
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measured_fraction_theta_full 0.656
_diffrn_measured_fraction_theta_max 0.656
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.48590
_diffrn_radiation_source         synchrotron
_diffrn_source_type              'DLS beamline I19'
_diffrn_ambient_pressure         1100000 #kpascals = 11kbar
_diffrn_measurement_specimen_support 'Diamond Anvil Cell'

_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                1384
_reflns_number_total             2051
_reflns_threshold_expression     >2σ(I)
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2011)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2011)
;
_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  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.927
_refine_diff_density_rms         0.226
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         2051
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1813
_refine_ls_R_factor_gt           0.1238
_refine_ls_restrained_S_all      1.092
_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)+(0.0000P)²+206.5763P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2272
_refine_ls_wR_factor_ref         0.2733
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  H4 of C4, H5 of C5, H6 of C6, H7 of C7
 At 1.5 times of:
  {H2A,H2B,H2C} of C2, {H1A,H1B,H1C} of C1, {H9A,H9B,H9C} of C9, {H10A,H10B,
  H10C} of C10
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7)
2.b Fitted hexagon refined as free rotating group:
 C3(C4,C5,C6,C7,C8)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.55623(9) 0.6209(2) 0.71998(14) 0.0309(7) Uani 1 1 d . . .
Cl1 Cl 0.4845(2) 0.8013(5) 0.5962(4) 0.0356(15) Uani 1 1 d . . .
Cl2 Cl 0.6483(2) 0.4968(5) 0.8346(4) 0.0348(15) Uani 1 1 d . . .
P1 P 0.5982(2) 0.6143(5) 0.5902(3) 0.0247(14) Uani 1 1 d . . .
P2 P 0.6038(2) 0.9057(5) 0.7606(3) 0.0282(15) Uani 1 1 d . . .
C1 C 0.6272(9) 0.398(2) 0.5789(14) 0.033(4) Uiso 1 1 d . . .
H1A H 0.6532 0.3685 0.6432 0.050 Uiso 1 1 calc R . .
H1B H 0.6419 0.4060 0.5261 0.050 Uiso 1 1 calc R . .
H1C H 0.6017 0.3038 0.5615 0.050 Uiso 1 1 calc R . .
C2 C 0.5576(9) 0.678(2) 0.4609(14) 0.036(4) Uiso 1 1 d . . .
H2A H 0.5283 0.5998 0.4387 0.054 Uiso 1 1 calc R . .
H2B H 0.5763 0.6664 0.4149 0.054 Uiso 1 1 calc R . .
H2C H 0.5467 0.8026 0.4610 0.054 Uiso 1 1 calc R . .
C3 C 0.6502(4) 0.7761(12) 0.6281(8) 0.025(3) Uiso 1 1 d G . .
C4 C 0.6880(5) 0.7702(11) 0.5846(7) 0.028(3) Uiso 1 1 d G . .
H4 H 0.6866 0.6830 0.5349 0.034 Uiso 1 1 calc R . .
C5 C 0.7280(4) 0.8945(13) 0.6153(8) 0.035(4) Uiso 1 1 d G . .
H5 H 0.7533 0.8905 0.5862 0.042 Uiso 1 1 calc R . .
C6 C 0.7301(4) 1.0247(13) 0.6895(8) 0.043(4) Uiso 1 1 d G . .
H6 H 0.7569 1.1078 0.7101 0.052 Uiso 1 1 calc R . .
C7 C 0.6923(5) 1.0306(11) 0.7330(7) 0.028(3) Uiso 1 1 d G . .
H7 H 0.6937 1.1177 0.7827 0.033 Uiso 1 1 calc R . .
C8 C 0.6523(4) 0.9063(12) 0.7023(8) 0.025(3) Uiso 1 1 d G . .
C9 C 0.5653(9) 1.110(2) 0.7138(14) 0.033(4) Uiso 1 1 d . . .
H9A H 0.5508 1.1057 0.6402 0.050 Uiso 1 1 calc R . .
H9B H 0.5863 1.2162 0.7347 0.050 Uiso 1 1 calc R . .
H9C H 0.5384 1.1142 0.7420 0.050 Uiso 1 1 calc R . .
C10 C 0.6386(10) 0.943(2) 0.8935(15) 0.040(4) Uiso 1 1 d . . .
H10A H 0.6577 1.0543 0.9016 0.060 Uiso 1 1 calc R . .
H10B H 0.6615 0.8429 0.9201 0.060 Uiso 1 1 calc R . .
H10C H 0.6153 0.9518 0.9303 0.060 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ge1 0.041(2) 0.0217(8) 0.0327(11) -0.0013(6) 0.0158(14) -0.0032(7)
Cl1 0.021(5) 0.036(2) 0.046(3) 0.0027(17) 0.007(4) -0.0007(17)
Cl2 0.035(5) 0.036(2) 0.034(3) 0.0036(16) 0.012(3) 0.0053(18)
P1 0.030(5) 0.0206(18) 0.022(2) -0.0012(14) 0.007(3) -0.0023(16)
P2 0.037(5) 0.0205(18) 0.029(3) -0.0058(14) 0.014(3) -0.0037(16)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
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
Ge1 Cl1 2.518(7) . ?
Ge1 Cl2 2.674(7) . ?
Ge1 P1 2.470(5) . ?
Ge1 P2 2.434(5) . ?
P1 C1 1.813(16) . ?
P1 C2 1.82(2) . ?
P1 C3 1.807(10) . ?
P2 C8 1.806(9) . ?
P2 C9 1.825(18) . ?
P2 C10 1.78(2) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.3900 . ?
C3 C8 1.3900 . ?
C4 H4 0.9300 . ?
C4 C5 1.3900 . ?
C5 H5 0.9300 . ?
C5 C6 1.3900 . ?
C6 H6 0.9300 . ?
C6 C7 1.3900 . ?
C7 H7 0.9300 . ?
C7 C8 1.3900 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?

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
Cl1 Ge1 Cl2 163.84(15) . . ?
P1 Ge1 Cl1 88.94(19) . . ?
P1 Ge1 Cl2 79.84(19) . . ?
P2 Ge1 Cl1 87.2(2) . . ?
P2 Ge1 Cl2 79.4(2) . . ?
P2 Ge1 P1 79.94(15) . . ?
C1 P1 Ge1 114.8(5) . . ?
C1 P1 C2 106.6(8) . . ?
C2 P1 Ge1 114.9(7) . . ?
C3 P1 Ge1 108.2(3) . . ?
C3 P1 C1 105.1(8) . . ?
C3 P1 C2 106.4(7) . . ?
C8 P2 Ge1 109.5(3) . . ?
C8 P2 C9 106.4(6) . . ?
C9 P2 Ge1 114.2(7) . . ?
C10 P2 Ge1 115.4(6) . . ?
C10 P2 C8 103.7(8) . . ?
C10 P2 C9 106.6(8) . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 P1 120.7(5) . . ?
C4 C3 C8 120.0 . . ?
C8 C3 P1 119.3(5) . . ?
C3 C4 H4 120.0 . . ?
C3 C4 C5 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C6 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 H6 120.0 . . ?
C5 C6 C7 120.0 . . ?
C7 C6 H6 120.0 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 C6 120.0 . . ?
C8 C7 H7 120.0 . . ?
C3 C8 P2 119.0(5) . . ?
C7 C8 P2 121.0(5) . . ?
C7 C8 C3 120.0 . . ?
P2 C9 H9A 109.5 . . ?
P2 C9 H9B 109.5 . . ?
P2 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P2 C10 H10A 109.5 . . ?
P2 C10 H10B 109.5 . . ?
P2 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ge1 P1 C3 C4 164.0(5) . . . . ?
Ge1 P1 C3 C8 -15.4(7) . . . . ?
Ge1 P2 C8 C3 13.5(7) . . . . ?
Ge1 P2 C8 C7 -164.4(5) . . . . ?
Cl1 Ge1 P1 C1 -138.8(9) . . . . ?
Cl1 Ge1 P1 C2 -14.6(6) . . . . ?
Cl1 Ge1 P1 C3 104.1(5) . . . . ?
Cl1 Ge1 P2 C8 -105.7(5) . . . . ?
Cl1 Ge1 P2 C9 13.5(5) . . . . ?
Cl1 Ge1 P2 C10 137.7(8) . . . . ?
Cl2 Ge1 P1 C1 52.9(9) . . . . ?
Cl2 Ge1 P1 C2 177.1(6) . . . . ?
Cl2 Ge1 P1 C3 -64.2(5) . . . . ?
Cl2 Ge1 P2 C8 65.1(5) . . . . ?
Cl2 Ge1 P2 C9 -175.7(6) . . . . ?
Cl2 Ge1 P2 C10 -51.5(8) . . . . ?
P1 Ge1 P2 C8 -16.3(5) . . . . ?
P1 Ge1 P2 C9 102.9(6) . . . . ?
P1 Ge1 P2 C10 -132.9(8) . . . . ?
P1 C3 C4 C5 -179.4(9) . . . . ?
P1 C3 C8 P2 1.5(8) . . . . ?
P1 C3 C8 C7 179.4(9) . . . . ?
P2 Ge1 P1 C1 133.8(9) . . . . ?
P2 Ge1 P1 C2 -102.0(6) . . . . ?
P2 Ge1 P1 C3 16.7(5) . . . . ?
C1 P1 C3 C4 40.8(9) . . . . ?
C1 P1 C3 C8 -138.6(7) . . . . ?
C2 P1 C3 C4 -72.0(9) . . . . ?
C2 P1 C3 C8 108.6(8) . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C4 C3 C8 P2 -177.9(8) . . . . ?
C4 C3 C8 C7 0.0 . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C5 C6 C7 C8 0.0 . . . . ?
C6 C7 C8 P2 177.8(8) . . . . ?
C6 C7 C8 C3 0.0 . . . . ?
C8 C3 C4 C5 0.0 . . . . ?
C9 P2 C8 C3 -110.4(9) . . . . ?
C9 P2 C8 C7 71.7(10) . . . . ?
C10 P2 C8 C3 137.3(8) . . . . ?
C10 P2 C8 C7 -40.6(9) . . . . ?

_database_code_depnum_ccdc_archive 'CCDC 977896'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gecl2diphos2
_audit_creation_date             2012-11-23
_audit_creation_method           
;
  Olex2 1.2
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
# start Validation Reply Form
_vrf_PLAT029_gecl2diphos2        
;
PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.434 
RESPONSE: Data are collected using a diamond anvil cell which has a limited 
opening angle which restricts the data accessible to measure.
This typically resulta in very low completeness although in this
case the wavelength of 0.48 angstrom improves completeness.
;

_chemical_name_common            ?
_chemical_name_systematic        
;
'Dichlorido(1,2-bis(dimethylphosphino)benzene)germanium(II)'
;
_chemical_formula_moiety         'C10 H16 Cl2 Ge P2'
_chemical_formula_sum            'C10 H16 Cl2 Ge P2'
_chemical_formula_weight         341.66
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0007 0.0007 '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'
Cl Cl 0.0777 0.0747 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.3342 0.9482 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0517 0.0444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z-1/2'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   27.691(16)
_cell_length_b                   7.225(3)
_cell_length_c                   13.704(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.00(3)
_cell_angle_gamma                90.00
_cell_volume                     2576(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    812
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       1400000 # kpascals = 14kbar
_cell_measurement_theta_max      18.4
_cell_measurement_theta_min      2.0
_exptl_absorpt_coefficient_mu    1.054
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.2256
_diffrn_reflns_av_unetI/netI     0.1529
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8513
_diffrn_reflns_theta_full        18.56
_diffrn_reflns_theta_max         18.56
_diffrn_reflns_theta_min         2.00
_diffrn_ambient_temperature      293
_diffrn_ambient_pressure         1400000 #kpascals = 14kbar
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.434
_diffrn_measured_fraction_theta_max 0.434
_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'Diamond Anvil Cell'
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.48590
_diffrn_source                   synchrotron
_diffrn_source_type              'DLS beamline I19'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                838
_reflns_number_total             1319
_reflns_threshold_expression     >2σ(I)
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2011)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2011)
;
_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  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.863
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.223
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         1319
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1954
_refine_ls_R_factor_gt           0.1138
_refine_ls_restrained_S_all      1.123
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0721P)²+171.5618P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2252
_refine_ls_wR_factor_ref         0.2981
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  H5 of C5, H4 of C4, H6 of C6, H7 of C7
 At 1.5 times of:
  {H9A,H9B,H9C} of C9, {H2A,H2B,H2C} of C2, {H1A,H1B,H1C} of C1, {H10A,H10B,
  H10C} of C10
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7)
2.b Fitted hexagon refined as free rotating group:
 C3(C4,C5,C6,C7,C8)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.55582(19) 0.6203(2) 0.72063(19) 0.050(2) Uani 1 1 d . . .
Cl1 Cl 0.4840(5) 0.8050(6) 0.5952(5) 0.070(7) Uani 1 1 d . . .
Cl2 Cl 0.6490(5) 0.4985(6) 0.8360(4) 0.048(5) Uani 1 1 d . . .
P1 P 0.5964(4) 0.6116(5) 0.5885(4) 0.043(5) Uani 1 1 d . . .
P2 P 0.6025(5) 0.9070(5) 0.7604(4) 0.043(5) Uani 1 1 d . . .
C1 C 0.6268(16) 0.394(2) 0.5762(17) 0.025(4) Uiso 1 1 d . . .
H1A H 0.6571 0.3757 0.6361 0.037 Uiso 1 1 calc R . .
H1B H 0.6361 0.3964 0.5149 0.037 Uiso 1 1 calc R . .
H1C H 0.6032 0.2936 0.5713 0.037 Uiso 1 1 calc R . .
C2 C 0.5612(18) 0.678(2) 0.4613(17) 0.032(4) Uiso 1 1 d . . .
H2A H 0.5297 0.6090 0.4371 0.048 Uiso 1 1 calc R . .
H2B H 0.5810 0.6534 0.4173 0.048 Uiso 1 1 calc R . .
H2C H 0.5537 0.8078 0.4598 0.048 Uiso 1 1 calc R . .
C3 C 0.6521(8) 0.7749(14) 0.6275(10) 0.026(4) Uiso 1 1 d G . .
C4 C 0.6908(8) 0.7681(14) 0.5846(10) 0.028(4) Uiso 1 1 d G . .
H4 H 0.6899 0.6787 0.5351 0.034 Uiso 1 1 calc R . .
C5 C 0.7310(8) 0.8948(16) 0.6156(11) 0.038(5) Uiso 1 1 d G . .
H5 H 0.7569 0.8902 0.5869 0.045 Uiso 1 1 calc R . .
C6 C 0.7324(8) 1.0283(16) 0.6895(11) 0.032(4) Uiso 1 1 d G . .
H6 H 0.7592 1.1131 0.7103 0.038 Uiso 1 1 calc R . .
C7 C 0.6936(8) 1.0351(14) 0.7324(10) 0.043(5) Uiso 1 1 d G . .
H7 H 0.6945 1.1245 0.7819 0.052 Uiso 1 1 calc R . .
C8 C 0.6535(8) 0.9084(15) 0.7014(11) 0.026(4) Uiso 1 1 d G . .
C9 C 0.5686(19) 1.117(2) 0.7149(19) 0.037(5) Uiso 1 1 d . . .
H9A H 0.5645 1.1346 0.6430 0.056 Uiso 1 1 calc R . .
H9B H 0.5876 1.2192 0.7548 0.056 Uiso 1 1 calc R . .
H9C H 0.5354 1.1112 0.7223 0.056 Uiso 1 1 calc R . .
C10 C 0.642(2) 0.950(3) 0.9008(19) 0.038(5) Uiso 1 1 d . . .
H10A H 0.6243 1.0338 0.9307 0.057 Uiso 1 1 calc R . .
H10B H 0.6746 1.0031 0.9049 0.057 Uiso 1 1 calc R . .
H10C H 0.6480 0.8350 0.9381 0.057 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ge1 0.104(7) 0.0203(9) 0.0363(14) -0.0002(8) 0.038(3) -0.0018(13)
Cl1 0.14(2) 0.030(2) 0.052(4) 0.000(2) 0.048(9) -0.001(4)
Cl2 0.079(18) 0.035(2) 0.033(3) 0.0040(19) 0.024(7) 0.000(3)
P1 0.091(17) 0.0218(19) 0.023(3) -0.0011(17) 0.029(7) -0.005(3)
P2 0.085(18) 0.0198(19) 0.029(3) -0.0030(17) 0.026(7) -0.001(3)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
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
Ge1 Cl1 2.521(11) . ?
Ge1 Cl2 2.673(12) . ?
Ge1 P1 2.437(7) . ?
Ge1 P2 2.404(8) . ?
P1 C1 1.82(2) . ?
P1 C2 1.75(3) . ?
P1 C3 1.867(18) . ?
P2 C8 1.850(17) . ?
P2 C9 1.78(3) . ?
P2 C10 1.89(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.3900 . ?
C3 C8 1.3900 . ?
C4 H4 0.9300 . ?
C4 C5 1.3900 . ?
C5 H5 0.9300 . ?
C5 C6 1.3900 . ?
C6 H6 0.9300 . ?
C6 C7 1.3900 . ?
C7 H7 0.9300 . ?
C7 C8 1.3900 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?

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
Cl1 Ge1 Cl2 162.7(3) . . ?
P1 Ge1 Cl1 87.9(3) . . ?
P1 Ge1 Cl2 80.4(3) . . ?
P2 Ge1 Cl1 86.4(3) . . ?
P2 Ge1 Cl2 79.3(3) . . ?
P2 Ge1 P1 80.9(2) . . ?
C1 P1 Ge1 115.9(6) . . ?
C1 P1 C3 102.2(14) . . ?
C2 P1 Ge1 119.5(14) . . ?
C2 P1 C1 105.2(11) . . ?
C2 P1 C3 103.7(12) . . ?
C3 P1 Ge1 108.4(4) . . ?
C8 P2 Ge1 109.7(4) . . ?
C8 P2 C10 100.3(16) . . ?
C9 P2 Ge1 118.5(15) . . ?
C9 P2 C8 103.4(12) . . ?
C9 P2 C10 105.7(12) . . ?
C10 P2 Ge1 117.0(8) . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 P1 122.5(7) . . ?
C4 C3 C8 120.0 . . ?
C8 C3 P1 117.5(7) . . ?
C3 C4 H4 120.0 . . ?
C3 C4 C5 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C6 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 H6 120.0 . . ?
C5 C6 C7 120.0 . . ?
C7 C6 H6 120.0 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 C6 120.0 . . ?
C8 C7 H7 120.0 . . ?
C3 C8 P2 118.6(7) . . ?
C7 C8 P2 121.3(7) . . ?
C7 C8 C3 120.0 . . ?
P2 C9 H9A 109.5 . . ?
P2 C9 H9B 109.5 . . ?
P2 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P2 C10 H10A 109.5 . . ?
P2 C10 H10B 109.4 . . ?
P2 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ge1 P1 C3 C4 162.9(6) . . . . ?
Ge1 P1 C3 C8 -18.0(9) . . . . ?
Ge1 P2 C8 C3 13.4(10) . . . . ?
Ge1 P2 C8 C7 -164.2(6) . . . . ?
Cl1 Ge1 P1 C1 -140.4(14) . . . . ?
Cl1 Ge1 P1 C2 -12.8(9) . . . . ?
Cl1 Ge1 P1 C3 105.5(7) . . . . ?
Cl1 Ge1 P2 C8 -106.2(7) . . . . ?
Cl1 Ge1 P2 C9 12.1(8) . . . . ?
Cl1 Ge1 P2 C10 140.5(15) . . . . ?
Cl2 Ge1 P1 C1 52.5(14) . . . . ?
Cl2 Ge1 P1 C2 -180.0(9) . . . . ?
Cl2 Ge1 P1 C3 -61.7(6) . . . . ?
Cl2 Ge1 P2 C8 64.2(7) . . . . ?
Cl2 Ge1 P2 C9 -177.6(8) . . . . ?
Cl2 Ge1 P2 C10 -49.2(15) . . . . ?
P1 Ge1 P2 C8 -17.7(7) . . . . ?
P1 Ge1 P2 C9 100.6(9) . . . . ?
P1 Ge1 P2 C10 -131.0(15) . . . . ?
P1 C3 C4 C5 179.1(11) . . . . ?
P1 C3 C8 P2 3.2(10) . . . . ?
P1 C3 C8 C7 -179.2(10) . . . . ?
P2 Ge1 P1 C1 133.0(15) . . . . ?
P2 Ge1 P1 C2 -99.5(9) . . . . ?
P2 Ge1 P1 C3 18.9(7) . . . . ?
C1 P1 C3 C4 40.0(10) . . . . ?
C1 P1 C3 C8 -140.8(9) . . . . ?
C2 P1 C3 C4 -69.2(13) . . . . ?
C2 P1 C3 C8 110.0(11) . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C4 C3 C8 P2 -177.6(10) . . . . ?
C4 C3 C8 C7 0.0 . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C5 C6 C7 C8 0.0 . . . . ?
C6 C7 C8 P2 177.6(10) . . . . ?
C6 C7 C8 C3 0.0 . . . . ?
C8 C3 C4 C5 0.0 . . . . ?
C9 P2 C8 C3 -113.9(14) . . . . ?
C9 P2 C8 C7 68.5(14) . . . . ?
C10 P2 C8 C3 137.1(9) . . . . ?
C10 P2 C8 C7 -40.4(10) . . . . ?

_database_code_depnum_ccdc_archive 'CCDC 977897'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gecl2diphos3
_audit_creation_date             2012-11-23
_audit_creation_method           
;
  Olex2 1.2
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;

# start Validation Reply Form
_vrf_PLAT029_gecl2diphos3        
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.427    
RESPONSE: Data are collected using a diamond anvil cell which has a limited 
opening angle which restricts the data accessible to measure.
This typically resulta in very low completeness although in this
case the wavelength of 0.48 angstrom improves completeness.
;

_chemical_name_common            ?
_chemical_name_systematic        
;
'Dichlorido(1,2-bis(dimethylphosphino)benzene)germanium(II)'
;
_chemical_formula_moiety         'C10 H16 Cl2 Ge P2'
_chemical_formula_sum            'C10 H16 Cl2 Ge P2'
_chemical_formula_weight         341.66
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0007 0.0007 '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'
Cl Cl 0.0777 0.0747 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.3342 0.9482 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0517 0.0444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z-1/2'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   27.380(8)
_cell_length_b                   7.0724(14)
_cell_length_c                   13.445(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.187(15)
_cell_angle_gamma                90.00
_cell_volume                     2443.6(9)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    927
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       3000000 # kpascals = 30kbar
_cell_measurement_theta_max      18.4
_cell_measurement_theta_min      2.0
_exptl_absorpt_coefficient_mu    1.111
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.1941
_diffrn_reflns_av_unetI/netI     0.1449
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7818
_diffrn_reflns_theta_full        18.44
_diffrn_reflns_theta_max         18.44
_diffrn_reflns_theta_min         2.04
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.427
_diffrn_measured_fraction_theta_max 0.427
_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_ambient_pressure         3000000 #kpascals = 30 kbar
_diffrn_measurement_specimen_support 'Diamond Anvil Cell'
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.48590
_diffrn_source                   synchrotron
_diffrn_source_type              'DLS beamline I19'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                839
_reflns_number_total             1209
_reflns_threshold_expression     >2σ(I)
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2011)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2011)
;
_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  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.994
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.232
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         1209
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1795
_refine_ls_R_factor_gt           0.1115
_refine_ls_restrained_S_all      1.114
_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)+(0.0000P)²+260.1917P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2177
_refine_ls_wR_factor_ref         0.2822
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  H7 of C7, H6 of C6, H5 of C5, H4 of C4
 At 1.5 times of:
  {H1a,H1b,H1c} of C1, {H2a,H2b,H2c} of C2, {H10a,H10b,H10c} of C10, {H9a,H9b,
  H9c} of C9
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7)
2.b Fitted hexagon refined as free rotating group:
 C3(C4,C5,C6,C7,C8)
2.c Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C2(H2a,H2b,H2c), C9(H9a,H9b,H9c), C10(H10a,H10b,H10c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.5543(2) 0.6194(2) 0.7219(2) 0.045(2) Uani 1 1 d . . .
Cl1 Cl 0.4835(5) 0.8096(6) 0.5935(5) 0.056(6) Uani 1 1 d . . .
Cl2 Cl 0.6486(5) 0.5027(6) 0.8374(5) 0.037(5) Uani 1 1 d . . .
P1 P 0.5974(5) 0.6062(6) 0.5884(4) 0.035(5) Uani 1 1 d . . .
P2 P 0.6014(5) 0.9139(6) 0.7601(4) 0.034(5) Uani 1 1 d . . .
C1 C 0.6342(18) 0.386(2) 0.5814(18) 0.021(4) Uiso 1 1 d . . .
H1A H 0.6685 0.3925 0.6336 0.031 Uiso 1 1 calc R . .
H1B H 0.6367 0.3760 0.5121 0.031 Uiso 1 1 calc R . .
H1C H 0.6162 0.2782 0.5948 0.031 Uiso 1 1 calc R . .
C2 C 0.563(2) 0.677(3) 0.461(2) 0.029(5) Uiso 1 1 d . . .
H2A H 0.5284 0.6239 0.4389 0.044 Uiso 1 1 calc R . .
H2B H 0.5802 0.6347 0.4139 0.044 Uiso 1 1 calc R . .
H2C H 0.5603 0.8127 0.4581 0.044 Uiso 1 1 calc R . .
C3 C 0.6521(8) 0.7730(15) 0.6271(10) 0.016(3) Uiso 1 1 d G . .
C4 C 0.6908(9) 0.7652(14) 0.5822(10) 0.021(4) Uiso 1 1 d G . .
H4 H 0.6896 0.6730 0.5321 0.026 Uiso 1 1 calc R . .
C5 C 0.7314(8) 0.8953(17) 0.6122(11) 0.024(4) Uiso 1 1 d G . .
H5 H 0.7573 0.8901 0.5821 0.028 Uiso 1 1 calc R . .
C6 C 0.7332(8) 1.0331(17) 0.6871(11) 0.030(5) Uiso 1 1 d G . .
H6 H 0.7603 1.1201 0.7072 0.036 Uiso 1 1 calc R . .
C7 C 0.6945(9) 1.0408(15) 0.7320(11) 0.035(5) Uiso 1 1 d G . .
H7 H 0.6957 1.1330 0.7822 0.042 Uiso 1 1 calc R . .
C8 C 0.6540(8) 0.9108(16) 0.7020(11) 0.018(4) Uiso 1 1 d G . .
C9 C 0.5634(18) 1.128(2) 0.7124(18) 0.021(4) Uiso 1 1 d . . .
H9A H 0.5489 1.1250 0.6365 0.032 Uiso 1 1 calc R . .
H9B H 0.5855 1.2365 0.7347 0.032 Uiso 1 1 calc R . .
H9C H 0.5358 1.1348 0.7411 0.032 Uiso 1 1 calc R . .
C10 C 0.6384(18) 0.965(2) 0.9012(18) 0.023(4) Uiso 1 1 d . . .
H10A H 0.6359 1.0969 0.9147 0.035 Uiso 1 1 calc R . .
H10B H 0.6742 0.9310 0.9169 0.035 Uiso 1 1 calc R . .
H10C H 0.6242 0.8922 0.9452 0.035 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ge1 0.100(8) 0.0153(9) 0.0303(15) 0.0017(8) 0.036(3) 0.0009(14)
Cl1 0.12(2) 0.022(2) 0.038(4) 0.000(2) 0.037(8) 0.002(4)
Cl2 0.060(17) 0.026(2) 0.026(3) -0.0001(19) 0.017(7) -0.007(3)
P1 0.079(17) 0.0166(19) 0.018(3) -0.0044(18) 0.028(7) -0.007(3)
P2 0.072(18) 0.016(2) 0.020(3) -0.0046(17) 0.024(7) -0.005(3)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
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
Ge1 Cl1 2.497(11) . ?
Ge1 Cl2 2.644(13) . ?
Ge1 P1 2.467(7) . ?
Ge1 P2 2.409(7) . ?
P1 C1 1.87(3) . ?
P1 C2 1.73(3) . ?
P1 C3 1.835(18) . ?
P2 C8 1.861(17) . ?
P2 C9 1.82(3) . ?
P2 C10 1.85(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.3900 . ?
C3 C8 1.3900 . ?
C4 H4 0.9300 . ?
C4 C5 1.3900 . ?
C5 H5 0.9300 . ?
C5 C6 1.3900 . ?
C6 H6 0.9300 . ?
C6 C7 1.3900 . ?
C7 H7 0.9300 . ?
C7 C8 1.3900 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?

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
Cl1 Ge1 Cl2 160.3(3) . . ?
P1 Ge1 Cl1 88.2(3) . . ?
P1 Ge1 Cl2 78.5(3) . . ?
P2 Ge1 Cl1 84.9(3) . . ?
P2 Ge1 Cl2 78.6(3) . . ?
P2 Ge1 P1 80.4(2) . . ?
C1 P1 Ge1 118.0(6) . . ?
C2 P1 Ge1 118.4(15) . . ?
C2 P1 C1 108.2(11) . . ?
C2 P1 C3 102.1(13) . . ?
C3 P1 Ge1 108.5(4) . . ?
C3 P1 C1 98.5(14) . . ?
C8 P2 Ge1 109.5(4) . . ?
C9 P2 Ge1 116.4(13) . . ?
C9 P2 C8 107.0(11) . . ?
C9 P2 C10 104.1(11) . . ?
C10 P2 Ge1 116.7(7) . . ?
C10 P2 C8 101.7(14) . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 P1 121.4(7) . . ?
C4 C3 C8 120.0 . . ?
C8 C3 P1 118.6(7) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C6 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 H6 120.0 . . ?
C5 C6 C7 120.0 . . ?
C7 C6 H6 120.0 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 C6 120.0 . . ?
C8 C7 H7 120.0 . . ?
C3 C8 P2 118.2(7) . . ?
C7 C8 P2 121.8(7) . . ?
C7 C8 C3 120.0 . . ?
P2 C9 H9A 109.5 . . ?
P2 C9 H9B 109.5 . . ?
P2 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P2 C10 H10A 109.5 . . ?
P2 C10 H10B 109.5 . . ?
P2 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ge1 P1 C3 C4 164.5(6) . . . . ?
Ge1 P1 C3 C8 -16.3(9) . . . . ?
Ge1 P2 C8 C3 15.0(10) . . . . ?
Ge1 P2 C8 C7 -164.6(6) . . . . ?
Cl1 Ge1 P1 C1 -145.7(15) . . . . ?
Cl1 Ge1 P1 C2 -12.1(10) . . . . ?
Cl1 Ge1 P1 C3 103.6(7) . . . . ?
Cl1 Ge1 P2 C8 -107.0(7) . . . . ?
Cl1 Ge1 P2 C9 14.5(7) . . . . ?
Cl1 Ge1 P2 C10 138.2(14) . . . . ?
Cl2 Ge1 P1 C1 48.9(15) . . . . ?
Cl2 Ge1 P1 C2 -177.5(10) . . . . ?
Cl2 Ge1 P1 C3 -61.9(7) . . . . ?
Cl2 Ge1 P2 C8 62.1(7) . . . . ?
Cl2 Ge1 P2 C9 -176.4(7) . . . . ?
Cl2 Ge1 P2 C10 -52.7(14) . . . . ?
P1 Ge1 P2 C8 -17.9(7) . . . . ?
P1 Ge1 P2 C9 103.6(8) . . . . ?
P1 Ge1 P2 C10 -132.7(14) . . . . ?
P1 C3 C4 C5 179.1(11) . . . . ?
P1 C3 C8 P2 1.2(10) . . . . ?
P1 C3 C8 C7 -179.2(10) . . . . ?
P2 Ge1 P1 C1 129.1(15) . . . . ?
P2 Ge1 P1 C2 -97.3(10) . . . . ?
P2 Ge1 P1 C3 18.4(7) . . . . ?
C1 P1 C3 C4 41.1(10) . . . . ?
C1 P1 C3 C8 -139.7(9) . . . . ?
C2 P1 C3 C4 -69.7(13) . . . . ?
C2 P1 C3 C8 109.5(12) . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C4 C3 C8 P2 -179.7(10) . . . . ?
C4 C3 C8 C7 0.0 . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C5 C6 C7 C8 0.0 . . . . ?
C6 C7 C8 P2 179.7(11) . . . . ?
C6 C7 C8 C3 0.0 . . . . ?
C8 C3 C4 C5 0.0 . . . . ?
C9 P2 C8 C3 -112.0(12) . . . . ?
C9 P2 C8 C7 68.4(13) . . . . ?
C10 P2 C8 C3 139.1(9) . . . . ?
C10 P2 C8 C7 -40.5(10) . . . . ?

_database_code_depnum_ccdc_archive 'CCDC 977898'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gecl2diphos7
_audit_creation_date             2012-11-27
_audit_creation_method           
;
  Olex2 1.2
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
# start Validation Reply Form
_vrf_PLAT029_gecl2diphos7        
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.617       
RESPONSE: Data are collected using a diamond anvil cell which has a limited 
opening angle which restricts the data accessible to measure.
This typically resulta in very low completeness although in this
case the wavelength of 0.48 angstrom improves completeness.
;

_chemical_name_common            ?
_chemical_name_systematic        
;
'Dichlorido(1,2-bis(dimethylphosphino)benzene)germanium(II)'
;
_chemical_formula_moiety         'C10 H16 Cl2 Ge P2'
_chemical_formula_sum            'C10 H16 Cl2 Ge P2'
_chemical_formula_weight         341.66
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0007 0.0007 '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'
Cl Cl 0.0777 0.0747 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.3342 0.9482 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0517 0.0444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z-1/2'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   26.91(4)
_cell_length_b                   6.962(8)
_cell_length_c                   13.249(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.30(7)
_cell_angle_gamma                90.00
_cell_volume                     2328(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       3800000 # kpascals = 38kbar
_cell_measurement_reflns_used    686
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      18.4
_exptl_absorpt_coefficient_mu    1.166
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.950
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ?
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.1241
_diffrn_reflns_av_unetI/netI     0.1354
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6215
_diffrn_reflns_theta_full        18.49
_diffrn_reflns_theta_max         18.49
_diffrn_reflns_theta_min         2.07
_diffrn_ambient_temperature      293(2)
_diffrn_source_type              'DLS beamline I19'
_diffrn_source                   synchrotron
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_ambient_pressure         3800000 #kpascals = 38kbar
_diffrn_measurement_specimen_support 'Diamond Anvil Cell'
_diffrn_measured_fraction_theta_full 0.617
_diffrn_measured_fraction_theta_max 0.617
_diffrn_radiation_wavelength     0.48590
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                1198
_reflns_number_total             1670
_reflns_threshold_expression     >2σ(I)
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2011)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2011)
;
_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  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.209
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         1670
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1471
_refine_ls_R_factor_gt           0.0969
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0001P)²+157.8856P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1691
_refine_ls_wR_factor_ref         0.2030
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H1A(0.034) H1B(0.034) H1C(0.034) H2A(0.033) H2B(0.033) H2C(0.033)
 H4(0.024) H5(0.026) H6(0.035) H7(0.025) H9A(0.031) H9B(0.031) H9C(0.031)
 H10A(0.039) H10B(0.039) H10C(0.039)
 Fixed X: H1A(0.6586) H1B(0.6419) H1C(0.6044) H2A(0.525) H2B(0.5755)
 H2C(0.5467) H4(0.6902) H5(0.7587) H6(0.7614) H7(0.6955) H9A(0.5484)
 H9B(0.5861) H9C(0.5364) H10A(0.6479) H10B(0.6704) H10C(0.6169)
 Fixed Y: H1A(0.3611) H1B(0.3896) H1C(0.2791) H2A(0.5966) H2B(0.6572)
 H2C(0.8069) H4(0.6659) H5(0.8879) H6(1.1244) H7(1.1389) H9A(1.1165)
 H9B(1.2359) H9C(1.1331) H10A(1.099) H10B(0.8892) H10C(0.9348)
 Fixed Z: H1A(0.6435) H1B(0.5188) H1C(0.5666) H2A(0.4321) H2B(0.4066)
 H2C(0.4558) H4(0.5314) H5(0.5811) H6(0.7062) H7(0.7817) H9A(0.6342)
 H9B(0.7307) H9C(0.7415) H10A(0.9092) H10B(0.9255) H10C(0.943)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.55436(8) 0.61798(16) 0.72241(11) 0.0184(5) Uani 1 1 d . . .
Cl1 Cl 0.48197(19) 0.8098(4) 0.5914(3) 0.0239(12) Uani 1 1 d . . .
Cl2 Cl 0.64875(18) 0.5022(4) 0.8376(3) 0.0189(11) Uani 1 1 d . . .
P1 P 0.59745(18) 0.6035(4) 0.5880(2) 0.0145(11) Uani 1 1 d . . .
P2 P 0.60284(19) 0.9137(4) 0.7615(3) 0.0158(11) Uani 1 1 d . . .
C1 C 0.6293(8) 0.3828(16) 0.5781(11) 0.022(3) Uiso 1 1 d . . .
H1A H 0.6586 0.3611 0.6435 0.034 Uiso 1 1 calc R . .
H1B H 0.6419 0.3896 0.5188 0.034 Uiso 1 1 calc R . .
H1C H 0.6044 0.2791 0.5666 0.034 Uiso 1 1 calc R . .
C2 C 0.5564(8) 0.6743(16) 0.4552(10) 0.022(3) Uiso 1 1 d . . .
H2A H 0.5250 0.5966 0.4321 0.033 Uiso 1 1 calc R . .
H2B H 0.5755 0.6572 0.4066 0.033 Uiso 1 1 calc R . .
H2C H 0.5467 0.8069 0.4558 0.033 Uiso 1 1 calc R . .
C3 C 0.6518(3) 0.7694(9) 0.6268(6) 0.018(2) Uiso 1 1 d G . .
C4 C 0.6912(4) 0.7607(9) 0.5816(6) 0.020(2) Uiso 1 1 d G . .
H4 H 0.6902 0.6659 0.5314 0.024 Uiso 1 1 calc R . .
C5 C 0.7323(3) 0.8937(10) 0.6113(7) 0.022(3) Uiso 1 1 d G . .
H5 H 0.7587 0.8879 0.5811 0.026 Uiso 1 1 calc R . .
C6 C 0.7339(3) 1.0354(10) 0.6863(7) 0.029(3) Uiso 1 1 d G . .
H6 H 0.7614 1.1244 0.7062 0.035 Uiso 1 1 calc R . .
C7 C 0.6945(4) 1.0441(9) 0.7316(6) 0.021(3) Uiso 1 1 d G . .
H7 H 0.6955 1.1389 0.7817 0.025 Uiso 1 1 calc R . .
C8 C 0.6534(3) 0.9111(10) 0.7018(6) 0.014(2) Uiso 1 1 d G . .
C9 C 0.5639(7) 1.1242(15) 0.7111(11) 0.021(2) Uiso 1 1 d . . .
H9A H 0.5484 1.1165 0.6342 0.031 Uiso 1 1 calc R . .
H9B H 0.5861 1.2359 0.7307 0.031 Uiso 1 1 calc R . .
H9C H 0.5364 1.1331 0.7415 0.031 Uiso 1 1 calc R . .
C10 C 0.6387(8) 0.9652(17) 0.9011(11) 0.026(3) Uiso 1 1 d . . .
H10A H 0.6479 1.0990 0.9092 0.039 Uiso 1 1 calc R . .
H10B H 0.6704 0.8892 0.9255 0.039 Uiso 1 1 calc R . .
H10C H 0.6169 0.9348 0.9430 0.039 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ge1 0.0174(17) 0.0164(6) 0.0220(8) -0.0002(5) 0.0075(10) -0.0018(5)
Cl1 0.018(4) 0.0239(16) 0.0242(19) 0.0020(11) 0.001(2) 0.0004(12)
Cl2 0.009(4) 0.0256(15) 0.0185(17) 0.0027(10) 0.001(2) 0.0031(12)
P1 0.015(4) 0.0148(14) 0.0123(17) -0.0019(10) 0.003(2) -0.0016(12)
P2 0.016(4) 0.0159(15) 0.0171(17) -0.0011(10) 0.007(2) 0.0004(12)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
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
Ge1 Cl1 2.499(5) . ?
Ge1 Cl2 2.596(6) . ?
Ge1 P1 2.441(4) . ?
Ge1 P2 2.396(4) . ?
P1 C1 1.786(13) . ?
P1 C2 1.791(16) . ?
P1 C3 1.793(8) . ?
P2 C8 1.795(7) . ?
P2 C9 1.790(14) . ?
P2 C10 1.800(16) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.3900 . ?
C3 C8 1.3900 . ?
C4 H4 0.9300 . ?
C4 C5 1.3900 . ?
C5 H5 0.9300 . ?
C5 C6 1.3900 . ?
C6 H6 0.9300 . ?
C6 C7 1.3900 . ?
C7 H7 0.9300 . ?
C7 C8 1.3900 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?

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
Cl1 Ge1 Cl2 160.41(12) . . ?
P1 Ge1 Cl1 88.19(16) . . ?
P1 Ge1 Cl2 78.50(16) . . ?
P2 Ge1 Cl1 85.74(16) . . ?
P2 Ge1 Cl2 77.96(15) . . ?
P2 Ge1 P1 80.37(12) . . ?
C1 P1 Ge1 116.8(4) . . ?
C1 P1 C2 108.2(6) . . ?
C1 P1 C3 102.2(7) . . ?
C2 P1 Ge1 114.7(5) . . ?
C2 P1 C3 105.6(6) . . ?
C3 P1 Ge1 108.1(3) . . ?
C8 P2 Ge1 109.6(3) . . ?
C8 P2 C10 103.7(7) . . ?
C9 P2 Ge1 114.7(6) . . ?
C9 P2 C8 106.2(5) . . ?
C9 P2 C10 104.8(6) . . ?
C10 P2 Ge1 116.8(4) . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 P1 121.1(4) . . ?
C4 C3 C8 120.0 . . ?
C8 C3 P1 118.9(4) . . ?
C3 C4 H4 120.0 . . ?
C3 C4 C5 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 H6 120.0 . . ?
C7 C6 C5 120.0 . . ?
C7 C6 H6 120.0 . . ?
C6 C7 H7 120.0 . . ?
C6 C7 C8 120.0 . . ?
C8 C7 H7 120.0 . . ?
C3 C8 P2 118.8(4) . . ?
C7 C8 P2 121.2(4) . . ?
C7 C8 C3 120.0 . . ?
P2 C9 H9A 109.5 . . ?
P2 C9 H9B 109.5 . . ?
P2 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P2 C10 H10A 109.5 . . ?
P2 C10 H10B 109.5 . . ?
P2 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ge1 P1 C3 C4 164.3(4) . . . . ?
Ge1 P1 C3 C8 -17.1(5) . . . . ?
Ge1 P2 C8 C3 12.8(5) . . . . ?
Ge1 P2 C8 C7 -165.4(4) . . . . ?
Cl1 Ge1 P1 C1 -141.8(7) . . . . ?
Cl1 Ge1 P1 C2 -13.7(5) . . . . ?
Cl1 Ge1 P1 C3 103.8(4) . . . . ?
Cl1 Ge1 P2 C8 -105.5(4) . . . . ?
Cl1 Ge1 P2 C9 13.8(4) . . . . ?
Cl1 Ge1 P2 C10 137.1(7) . . . . ?
Cl2 Ge1 P1 C1 52.7(7) . . . . ?
Cl2 Ge1 P1 C2 -179.2(5) . . . . ?
Cl2 Ge1 P1 C3 -61.8(4) . . . . ?
Cl2 Ge1 P2 C8 63.6(4) . . . . ?
Cl2 Ge1 P2 C9 -177.2(4) . . . . ?
Cl2 Ge1 P2 C10 -53.9(7) . . . . ?
P1 Ge1 P2 C8 -16.6(4) . . . . ?
P1 Ge1 P2 C9 102.7(4) . . . . ?
P1 Ge1 P2 C10 -134.1(7) . . . . ?
P1 C3 C4 C5 178.6(7) . . . . ?
P1 C3 C8 P2 3.2(6) . . . . ?
P1 C3 C8 C7 -178.6(7) . . . . ?
P2 Ge1 P1 C1 132.2(7) . . . . ?
P2 Ge1 P1 C2 -99.6(5) . . . . ?
P2 Ge1 P1 C3 17.8(4) . . . . ?
C1 P1 C3 C4 40.5(6) . . . . ?
C1 P1 C3 C8 -140.9(6) . . . . ?
C2 P1 C3 C4 -72.6(7) . . . . ?
C2 P1 C3 C8 106.0(6) . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C4 C3 C8 P2 -178.2(6) . . . . ?
C4 C3 C8 C7 0.0 . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C5 C6 C7 C8 0.0 . . . . ?
C6 C7 C8 P2 178.1(6) . . . . ?
C6 C7 C8 C3 0.0 . . . . ?
C8 C3 C4 C5 0.0 . . . . ?
C9 P2 C8 C3 -111.7(7) . . . . ?
C9 P2 C8 C7 70.2(7) . . . . ?
C10 P2 C8 C3 138.1(6) . . . . ?
C10 P2 C8 C7 -40.0(6) . . . . ?

_database_code_depnum_ccdc_archive 'CCDC 977899'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gebr2diphos9

_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2013-01-16

# start Validation Reply Form
_vrf_PLAT029_gebr2diphos9        
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.279     
RESPONSE: Data are collected using a diamond anvil cell which has a limited 
opening angle which restricts the data accessible to measure.
This resulting low completeness is typical of these studies.
;
_chemical_name_systematic        
;
 Dibromo(1,2-bis(dimethylphosphino)benzene-P,P')germanium(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H16 Br2 Ge P2'
_chemical_formula_sum            'C10 H16 Br2 Ge P2'
_chemical_formula_weight         430.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0032 0.0015 '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'
Br Br -0.1750 2.4304 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.2186 1.7697 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0990 0.0908 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'

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'

_cell_length_a                   24.30(13)
_cell_length_b                   6.83(3)
_cell_length_c                   13.37(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.3(3)
_cell_angle_gamma                90.00
_cell_volume                     2217(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       9400000 # kpascals = 94kbar
_cell_measurement_reflns_used    473
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      28.7

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1664
_exptl_absorpt_coefficient_mu    9.423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  1.000
_exptl_absorpt_correction_T_max  0.439
_exptl_absorpt_process_details   
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;

_diffrn_ambient_temperature      293
_diffrn_ambient_pressure         9400000 #kpascals = 94kbar
_diffrn_measurement_specimen_support 'Diamond Anvil Cell'
_diffrn_radiation_wavelength     0.68890
_diffrn_radiation_type           synchrotron
_diffrn_source_type              'DLS beamline I19'
_diffrn_source                   synchrotron
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'


_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3965
_diffrn_reflns_av_R_equivalents  0.0863
_diffrn_reflns_av_sigmaI/netI    0.0836
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         28.96
_reflns_number_total             903
_reflns_number_gt                630
_reflns_threshold_expression     I>2/sigma(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;

_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0735P)²+335.2057P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         903
_refine_ls_number_parameters     74
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1391
_refine_ls_R_factor_gt           0.1005
_refine_ls_wR_factor_ref         0.2729
_refine_ls_wR_factor_gt          0.2415
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_restrained_S_all      1.121
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.356(4) -0.460(4) 0.678(2) 0.037(7) Uiso 1 1 d . . .
H1A H 0.3335 -0.3496 0.6602 0.056 Uiso 1 1 calc R . .
H1B H 0.3336 -0.5720 0.6892 0.056 Uiso 1 1 calc R . .
H1C H 0.3806 -0.4871 0.6251 0.056 Uiso 1 1 calc R . .
C2 C 0.437(3) -0.627(4) 0.8208(18) 0.028(6) Uiso 1 1 d . . .
H2A H 0.4590 -0.6108 0.8815 0.042 Uiso 1 1 calc R . .
H2B H 0.4605 -0.6532 0.7664 0.042 Uiso 1 1 calc R . .
H2C H 0.4120 -0.7346 0.8283 0.042 Uiso 1 1 calc R . .
C3 C 0.3421(15) -0.410(3) 0.8819(11) 0.030(6) Uiso 1 1 d G . .
C4 C 0.3007(16) -0.550(2) 0.8719(10) 0.029(6) Uiso 1 1 d G . .
H4 H 0.2985 -0.6301 0.8156 0.035 Uiso 1 1 calc R . .
C5 C 0.2626(15) -0.570(2) 0.9461(12) 0.028(6) Uiso 1 1 d G . .
H5 H 0.2349 -0.6637 0.9394 0.033 Uiso 1 1 calc R . .
C6 C 0.2660(15) -0.451(3) 1.0302(11) 0.032(7) Uiso 1 1 d G . .
H6 H 0.2405 -0.4640 1.0798 0.039 Uiso 1 1 calc R . .
C7 C 0.3074(16) -0.311(2) 1.0401(10) 0.033(7) Uiso 1 1 d G . .
H7 H 0.3096 -0.2306 1.0964 0.039 Uiso 1 1 calc R . .
C8 C 0.3455(15) -0.291(3) 0.9660(12) 0.024(6) Uiso 1 1 d G . .
C9 C 0.447(3) -0.178(4) 1.0849(15) 0.021(5) Uiso 1 1 d . . .
H9A H 0.4755 -0.0812 1.0938 0.031 Uiso 1 1 calc R . .
H9B H 0.4636 -0.3038 1.0742 0.031 Uiso 1 1 calc R . .
H9C H 0.4257 -0.1832 1.1437 0.031 Uiso 1 1 calc R . .
C10 C 0.376(3) 0.111(4) 1.005(2) 0.034(7) Uiso 1 1 d . . .
H10A H 0.4050 0.2060 1.0057 0.051 Uiso 1 1 calc R . .
H10B H 0.3610 0.1039 1.0705 0.051 Uiso 1 1 calc R . .
H10C H 0.3474 0.1497 0.9573 0.051 Uiso 1 1 calc R . .
P1 P 0.3976(9) -0.4027(9) 0.7948(5) 0.053(14) Uani 1 1 d . . .
P2 P 0.4010(9) -0.1122(10) 0.9730(5) 0.062(14) Uani 1 1 d . . .
Ge1 Ge 0.4426(4) -0.1019(4) 0.81154(19) 0.067(6) Uani 1 1 d . . .
Br1 Br 0.5185(4) -0.3070(4) 0.8985(2) 0.082(6) Uani 1 1 d . . .
Br2 Br 0.3300(4) 0.0042(4) 0.75793(18) 0.081(6) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.11(4) 0.013(3) 0.033(3) -0.001(2) -0.007(7) -0.009(6)
P2 0.14(4) 0.017(3) 0.025(3) -0.002(2) 0.003(7) 0.004(6)
Ge1 0.160(18) 0.0134(12) 0.0296(13) 0.0006(9) 0.014(3) -0.003(3)
Br1 0.185(18) 0.0202(12) 0.0404(15) 0.0007(10) 0.007(3) -0.001(3)
Br2 0.195(18) 0.0203(12) 0.0265(12) -0.0008(9) 0.004(3) 0.004(3)

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

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 P1 1.86(5) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 P1 1.83(5) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.3900 . ?
C3 C8 1.3900 . ?
C3 P1 1.82(3) . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 C6 1.3900 . ?
C5 H5 0.9300 . ?
C6 C7 1.3900 . ?
C6 H6 0.9300 . ?
C7 C8 1.3900 . ?
C7 H7 0.9300 . ?
C8 P2 1.82(3) . ?
C9 P2 1.89(5) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 P2 1.71(4) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
P1 Ge1 2.333(15) . ?
P2 Ge1 2.422(17) . ?
Ge1 Br1 2.559(14) . ?

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
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 120.0 . . ?
C4 C3 P1 120.7(12) . . ?
C8 C3 P1 118.7(12) . . ?
C3 C4 C5 120.0 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 120.0 . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C8 C7 C6 120.0 . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C3 120.0 . . ?
C7 C8 P2 122.9(11) . . ?
C3 C8 P2 117.1(11) . . ?
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 . . ?
C3 P1 C2 104(2) . . ?
C3 P1 C1 98(3) . . ?
C2 P1 C1 104.1(19) . . ?
C3 P1 Ge1 108.7(7) . . ?
C2 P1 Ge1 119(2) . . ?
C1 P1 Ge1 120.0(12) . . ?
C10 P2 C8 110(3) . . ?
C10 P2 C9 102.8(19) . . ?
C8 P2 C9 107.3(16) . . ?
C10 P2 Ge1 111.4(13) . . ?
C8 P2 Ge1 108.0(7) . . ?
C9 P2 Ge1 117(2) . . ?
P1 Ge1 P2 81.3(5) . . ?
P1 Ge1 Br1 83.6(6) . . ?
P2 Ge1 Br1 84.2(6) . . ?

_diffrn_measured_fraction_theta_max 0.279
_diffrn_reflns_theta_full        28.96
_diffrn_measured_fraction_theta_full 0.279
_refine_diff_density_max         0.900
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.232
_database_code_depnum_ccdc_archive 'CCDC 977912'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_GeBr2diphos1
_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2012-03-26

# start Validation Reply Form
_vrf_PLAT029_GeBr2diphos1        
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.287      
RESPONSE: Data are collected using a diamond anvil cell which has a limited 
opening angle which restricts the data accessible to measure.
This resulting low completeness is typical of these studies.
;

_chemical_name_systematic        
;
 Dibromo(1,2-bis(dimethylphosphino)benzene-P,P')germanium(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H16 Br2 Ge P2'
_chemical_formula_sum            'C10 H16 Br2 Ge P2'
_chemical_formula_weight         430.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0028 0.0015 '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'
Br Br -0.1853 2.3459 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1952 1.7169 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0974 0.0893 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'

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'

_cell_length_a                   29.46(4)
_cell_length_b                   7.628(9)
_cell_length_c                   14.510(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.334(18)
_cell_angle_gamma                90.00
_cell_volume                     3037(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    293
_cell_measurement_pressure       100 # kpascals = 1bar
_cell_measurement_reflns_used    640
_cell_measurement_theta_min      2.7
_cell_measurement_theta_max      28.5


_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.883
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1664
_exptl_absorpt_coefficient_mu    6.879
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  1.000
_exptl_absorpt_correction_T_max  0.719
_exptl_absorpt_process_details   
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2011)
;


_diffrn_ambient_temperature      293
_diffrn_ambient_pressure         100 #kpascals = 1bar
_diffrn_measurement_specimen_support 'Diamond Anvil Cell'
_diffrn_radiation_wavelength     0.68890
_diffrn_radiation_type           synchrotron
_diffrn_source_type              'DLS beamline I19'
_diffrn_source                   synchrotron
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'


_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5764
_diffrn_reflns_av_R_equivalents  0.0773
_diffrn_reflns_av_sigmaI/netI    0.0860
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.75
_diffrn_reflns_theta_max         29.30
_reflns_number_total             1312
_reflns_number_gt                909
_reflns_threshold_expression     I>2/sigma(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+93.9316P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1312
_refine_ls_number_parameters     74
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1311
_refine_ls_R_factor_gt           0.0792
_refine_ls_wR_factor_ref         0.1904
_refine_ls_wR_factor_gt          0.1522
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_restrained_S_all      1.156
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.002

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3729(14) 0.4147(17) 0.9133(13) 0.036(3) Uiso 1 1 d . . .
H1A H 0.3533 0.3729 0.8486 0.054 Uiso 1 1 calc R . .
H1B H 0.3526 0.4320 0.9515 0.054 Uiso 1 1 calc R . .
H1C H 0.3977 0.3301 0.9457 0.054 Uiso 1 1 calc R . .
C2 C 0.4368(16) 0.683(2) 1.0270(14) 0.048(4) Uiso 1 1 d . . .
H2A H 0.4530 0.7925 1.0273 0.072 Uiso 1 1 calc R . .
H2B H 0.4607 0.5939 1.0566 0.072 Uiso 1 1 calc R . .
H2C H 0.4159 0.6949 1.0641 0.072 Uiso 1 1 calc R . .
C3 C 0.3509(7) 0.7809(12) 0.8632(8) 0.035(3) Uiso 1 1 d G . .
C4 C 0.3156(8) 0.7797(12) 0.9058(9) 0.045(4) Uiso 1 1 d G . .
H4 H 0.3167 0.6960 0.9532 0.054 Uiso 1 1 calc R . .
C5 C 0.2784(7) 0.9038(14) 0.8775(10) 0.051(4) Uiso 1 1 d G . .
H5 H 0.2548 0.9030 0.9060 0.062 Uiso 1 1 calc R . .
C6 C 0.2767(7) 1.0289(14) 0.8066(9) 0.062(5) Uiso 1 1 d G . .
H6 H 0.2518 1.1119 0.7877 0.075 Uiso 1 1 calc R . .
C7 C 0.3120(8) 1.0301(12) 0.7641(8) 0.049(4) Uiso 1 1 d G . .
H7 H 0.3108 1.1139 0.7167 0.059 Uiso 1 1 calc R . .
C8 C 0.3491(7) 0.9061(12) 0.7924(8) 0.035(3) Uiso 1 1 d G . .
C9 C 0.4310(17) 1.099(2) 0.7769(16) 0.055(5) Uiso 1 1 d . . .
H9A H 0.4493 1.0912 0.8466 0.082 Uiso 1 1 calc R . .
H9B H 0.4096 1.1980 0.7636 0.082 Uiso 1 1 calc R . .
H9C H 0.4530 1.1114 0.7421 0.082 Uiso 1 1 calc R . .
C10 C 0.3650(16) 0.938(2) 0.6068(14) 0.048(4) Uiso 1 1 d . . .
H10A H 0.3447 0.8390 0.5775 0.072 Uiso 1 1 calc R . .
H10B H 0.3886 0.9535 0.5763 0.072 Uiso 1 1 calc R . .
H10C H 0.3452 1.0412 0.5970 0.072 Uiso 1 1 calc R . .
Br1 Br 0.34848(18) 0.4915(2) 0.65691(15) 0.066(3) Uani 1 1 d . . .
Br2 Br 0.5161(2) 0.7975(2) 0.90356(18) 0.071(3) Uani 1 1 d . . .
Ge1 Ge 0.44099(17) 0.62475(19) 0.77808(15) 0.048(3) Uani 1 1 d . . .
P1 P 0.4014(4) 0.6229(4) 0.9022(3) 0.039(6) Uani 1 1 d . . .
P2 P 0.3954(4) 0.9004(5) 0.7359(4) 0.040(7) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.106(10) 0.0498(9) 0.0468(14) -0.0038(8) 0.035(3) -0.0047(16)
Br2 0.098(11) 0.0533(10) 0.0643(17) 0.0007(9) 0.034(4) 0.0006(18)
Ge1 0.073(9) 0.0333(8) 0.0459(14) 0.0004(7) 0.030(3) 0.0065(14)
P1 0.05(2) 0.0313(17) 0.032(3) 0.0042(16) 0.014(7) 0.011(3)
P2 0.05(2) 0.0351(19) 0.043(3) 0.0081(17) 0.023(8) 0.012(3)

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

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 P1 1.83(2) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 P1 1.79(3) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.3900 . ?
C3 C8 1.3900 . ?
C3 P1 1.837(17) . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 C6 1.3900 . ?
C5 H5 0.9300 . ?
C6 C7 1.3900 . ?
C6 H6 0.9300 . ?
C7 C8 1.3900 . ?
C7 H7 0.9300 . ?
C8 P2 1.830(16) . ?
C9 P2 1.81(3) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 P2 1.78(2) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
Br1 Ge1 2.840(7) . ?
Br2 Ge1 2.649(6) . ?
Ge1 P2 2.450(7) . ?
Ge1 P1 2.477(7) . ?

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
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 120.0 . . ?
C4 C3 P1 120.8(6) . . ?
C8 C3 P1 119.2(6) . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C7 C6 C5 120.0 . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C8 120.0 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C3 120.0 . . ?
C7 C8 P2 121.2(6) . . ?
C3 C8 P2 118.8(6) . . ?
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 . . ?
P2 Ge1 P1 80.0(2) . . ?
P2 Ge1 Br2 89.4(3) . . ?
P1 Ge1 Br2 90.0(2) . . ?
P2 Ge1 Br1 80.6(3) . . ?
P1 Ge1 Br1 81.3(3) . . ?
Br2 Ge1 Br1 167.71(15) . . ?
C2 P1 C1 104.5(9) . . ?
C2 P1 C3 104.6(11) . . ?
C1 P1 C3 104.5(13) . . ?
C2 P1 Ge1 118.6(13) . . ?
C1 P1 Ge1 114.9(6) . . ?
C3 P1 Ge1 108.4(4) . . ?
C10 P2 C9 102.8(11) . . ?
C10 P2 C8 107.2(15) . . ?
C9 P2 C8 105.7(11) . . ?
C10 P2 Ge1 114.9(7) . . ?
C9 P2 Ge1 115.7(14) . . ?
C8 P2 Ge1 109.8(4) . . ?

_diffrn_measured_fraction_theta_max 0.287
_diffrn_reflns_theta_full        29.30
_diffrn_measured_fraction_theta_full 0.287
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.131
_database_code_depnum_ccdc_archive 'CCDC 977913'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gebr2diphos2new

_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2012-08-24

# start Validation Reply Form
_vrf_PLAT029_gebr2diphos2new     
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.287      
RESPONSE: Data are collected using a diamond anvil cell which has a limited 
opening angle which restricts the data accessible to measure.
This resulting low completeness is typical of these studies.
;

_chemical_name_systematic        
;
 Dibromo(1,2-bis(dimethylphosphino)benzene-P,P')germanium(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H16 Br2 Ge P2'
_chemical_formula_sum            'C10 H16 Br2 Ge P2'
_chemical_formula_weight         430.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0028 0.0015 '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'
Br Br -0.1853 2.3459 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1952 1.7169 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0974 0.0893 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'

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'

_cell_length_a                   29.22(4)
_cell_length_b                   7.578(8)
_cell_length_c                   14.434(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.13(2)
_cell_angle_gamma                90.00
_cell_volume                     2981(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       200000 # kpascals = 2kbar
_cell_measurement_reflns_used    603
_cell_measurement_theta_min      2.7
_cell_measurement_theta_max      28.6

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.918
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1664
_exptl_absorpt_coefficient_mu    7.008
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  1.000
_exptl_absorpt_correction_T_max  0.661
_exptl_absorpt_process_details   
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2011)
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293
_diffrn_ambient_pressure         200000 #kpascals = 2kbar
_diffrn_measurement_specimen_support 'Diamond Anvil Cell'
_diffrn_radiation_wavelength     0.68890
_diffrn_radiation_type           synchrotron
_diffrn_source_type              'DLS beamline I19'
_diffrn_source                   synchrotron
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'


_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5520
_diffrn_reflns_av_R_equivalents  0.1146
_diffrn_reflns_av_sigmaI/netI    0.1540
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.79
_diffrn_reflns_theta_max         30.35
_reflns_number_total             1292
_reflns_number_gt                608
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1291
_refine_ls_number_parameters     74
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1830
_refine_ls_R_factor_gt           0.0909
_refine_ls_wR_factor_ref         0.3490
_refine_ls_wR_factor_gt          0.2416
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.368(2) 0.415(3) 0.909(2) 0.038(6) Uiso 1 1 d . . .
H1A H 0.3489 0.3767 0.8429 0.057 Uiso 1 1 calc R . .
H1B H 0.3470 0.4374 0.9453 0.057 Uiso 1 1 calc R . .
H1C H 0.3915 0.3253 0.9418 0.057 Uiso 1 1 calc R . .
C2 C 0.442(3) 0.681(3) 1.030(2) 0.058(8) Uiso 1 1 d . . .
H2A H 0.4575 0.7914 1.0290 0.087 Uiso 1 1 calc R . .
H2B H 0.4661 0.5907 1.0559 0.087 Uiso 1 1 calc R . .
H2C H 0.4223 0.6906 1.0712 0.087 Uiso 1 1 calc R . .
C3 C 0.3507(12) 0.7799(17) 0.8626(13) 0.033(5) Uiso 1 1 d G . .
C4 C 0.3152(13) 0.7803(19) 0.9059(13) 0.055(8) Uiso 1 1 d G . .
H4 H 0.3160 0.6954 0.9530 0.066 Uiso 1 1 calc R . .
C5 C 0.2785(12) 0.908(2) 0.8789(15) 0.062(8) Uiso 1 1 d G . .
H5 H 0.2548 0.9080 0.9079 0.075 Uiso 1 1 calc R . .
C6 C 0.2773(12) 1.035(2) 0.8085(14) 0.063(8) Uiso 1 1 d G . .
H6 H 0.2528 1.1199 0.7904 0.075 Uiso 1 1 calc R . .
C7 C 0.3128(12) 1.0342(17) 0.7652(13) 0.043(6) Uiso 1 1 d G . .
H7 H 0.3119 1.1192 0.7181 0.051 Uiso 1 1 calc R . .
C8 C 0.3494(12) 0.9068(18) 0.7922(13) 0.034(5) Uiso 1 1 d G . .
C9 C 0.428(2) 1.101(3) 0.776(2) 0.039(6) Uiso 1 1 d . . .
H9A H 0.4458 1.0950 0.8463 0.059 Uiso 1 1 calc R . .
H9B H 0.4052 1.1982 0.7622 0.059 Uiso 1 1 calc R . .
H9C H 0.4502 1.1188 0.7419 0.059 Uiso 1 1 calc R . .
C10 C 0.359(3) 0.934(3) 0.602(2) 0.043(6) Uiso 1 1 d . . .
H10A H 0.3399 0.8312 0.5768 0.064 Uiso 1 1 calc R . .
H10B H 0.3813 0.9527 0.5670 0.064 Uiso 1 1 calc R . .
H10C H 0.3384 1.0352 0.5935 0.064 Uiso 1 1 calc R . .
Br1 Br 0.3488(3) 0.4940(3) 0.6555(2) 0.088(5) Uani 1 1 d . . .
Br2 Br 0.5168(3) 0.8010(3) 0.9045(3) 0.106(6) Uani 1 1 d . . .
Ge1 Ge 0.4408(3) 0.6256(3) 0.7767(3) 0.093(5) Uani 1 1 d . . .
P1 P 0.4013(8) 0.6216(7) 0.9019(7) 0.112(13) Uani 1 1 d . . .
P2 P 0.3954(7) 0.9038(7) 0.7356(6) 0.046(11) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.178(16) 0.0463(14) 0.057(2) -0.0038(12) 0.065(6) -0.003(3)
Br2 0.215(19) 0.0465(16) 0.072(3) 0.0014(13) 0.070(7) 0.005(3)
Ge1 0.213(16) 0.0286(13) 0.060(2) -0.0006(11) 0.079(6) 0.001(2)
P1 0.28(4) 0.027(3) 0.067(6) 0.001(3) 0.108(14) 0.001(6)
P2 0.07(3) 0.030(3) 0.036(5) 0.004(2) 0.014(11) -0.003(5)

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

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 P1 1.86(4) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 P1 1.85(5) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.3900 . ?
C3 C8 1.3900 . ?
C3 P1 1.83(3) . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 C6 1.3900 . ?
C5 H5 0.9300 . ?
C6 C7 1.3900 . ?
C6 H6 0.9300 . ?
C7 C8 1.3900 . ?
C7 H7 0.9300 . ?
C8 P2 1.81(3) . ?
C9 P2 1.76(4) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 P2 1.85(4) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
Br1 Ge1 2.810(11) . ?
Br2 Ge1 2.672(9) . ?
Ge1 P2 2.449(12) . ?
Ge1 P1 2.470(12) . ?

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
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 120.0 . . ?
C4 C3 P1 120.9(10) . . ?
C8 C3 P1 119.0(10) . . ?
C3 C4 C5 120.0 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C7 C6 C5 120.0 . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C8 120.0 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C3 120.0 . . ?
C7 C8 P2 120.4(10) . . ?
C3 C8 P2 119.6(10) . . ?
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 . . ?
P2 Ge1 P1 80.3(4) . . ?
P2 Ge1 Br2 89.0(4) . . ?
P1 Ge1 Br2 89.5(4) . . ?
P2 Ge1 Br1 80.8(4) . . ?
P1 Ge1 Br1 81.7(5) . . ?
Br2 Ge1 Br1 167.5(2) . . ?
C3 P1 C2 107.6(17) . . ?
C3 P1 C1 101(2) . . ?
C2 P1 C1 107.8(15) . . ?
C3 P1 Ge1 107.7(6) . . ?
C2 P1 Ge1 115(2) . . ?
C1 P1 Ge1 116.1(9) . . ?
C9 P2 C8 103.8(16) . . ?
C9 P2 C10 106.0(15) . . ?
C8 P2 C10 104(2) . . ?
C9 P2 Ge1 118(2) . . ?
C8 P2 Ge1 109.2(6) . . ?
C10 P2 Ge1 114.6(10) . . ?

_diffrn_measured_fraction_theta_max 0.287
_diffrn_reflns_theta_full        30.35
_diffrn_measured_fraction_theta_full 0.287
_refine_diff_density_max         1.242
_refine_diff_density_min         -1.571
_refine_diff_density_rms         0.293
_database_code_depnum_ccdc_archive 'CCDC 977914'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gebr2diphos3_multi_aug24

_audit_creation_method           SHELXL-97

# start Validation Reply Form
_vrf_PLAT029_gebr2diphos3_multi_aug24 
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.289      
RESPONSE: Data are collected using a diamond anvil cell which has a limited 
opening angle which restricts the data accessible to measure.
This resulting low completeness is typical of these studies.
;

_chemical_name_systematic        
;
 Dibromo(1,2-bis(dimethylphosphino)benzene-P,P')germanium(II)
;

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H16 Br2 Ge P2'
_chemical_formula_sum            'C10 H16 Br2 Ge P2'
_chemical_formula_weight         430.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0032 0.0015 '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'
Br Br -0.1750 2.4304 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.2186 1.7697 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0990 0.0908 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'

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'

_cell_length_a                   28.41(3)
_cell_length_b                   7.339(5)
_cell_length_c                   14.008(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.53(2)
_cell_angle_gamma                90.00
_cell_volume                     2717(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       1100000 # kpascals = 11kbar
_cell_measurement_reflns_used    556
_cell_measurement_theta_min      2.8
_cell_measurement_theta_max      29.1

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.105
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1664
_exptl_absorpt_coefficient_mu    7.690
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.439
_exptl_absorpt_process_details   
;
Rigaku CrystalClear-SM Expert 2.0 r5
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293
_diffrn_ambient_pressure         1100000 #kpascals = 11kbar
_diffrn_measurement_specimen_support 'Diamond Anvil Cell'
_diffrn_radiation_wavelength     0.68890
_diffrn_radiation_type           synchrotron
_diffrn_source_type              'DLS beamline I19'
_diffrn_source                   synchrotron
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'


_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_method       'profile data from ω-scans'

_diffrn_reflns_number            4632
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_sigmaI/netI    0.0923
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.79
_diffrn_reflns_theta_max         29.11
_reflns_number_total             1159
_reflns_number_gt                742
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1159
_refine_ls_number_parameters     74
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1468
_refine_ls_R_factor_gt           0.0838
_refine_ls_wR_factor_ref         0.3289
_refine_ls_wR_factor_gt          0.2366
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_restrained_S_all      1.179
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.370(2) 0.399(2) 0.9089(18) 0.024(4) Uiso 1 1 d . . .
H1A H 0.3500 0.3594 0.8406 0.036 Uiso 1 1 calc R . .
H1B H 0.3486 0.4156 0.9475 0.036 Uiso 1 1 calc R . .
H1C H 0.3952 0.3082 0.9417 0.036 Uiso 1 1 calc R . .
C2 C 0.439(2) 0.676(3) 1.031(2) 0.033(5) Uiso 1 1 d . . .
H2A H 0.4554 0.7907 1.0315 0.049 Uiso 1 1 calc R . .
H2B H 0.4641 0.5839 1.0606 0.049 Uiso 1 1 calc R . .
H2C H 0.4178 0.6868 1.0708 0.049 Uiso 1 1 calc R . .
C3 C 0.3497(10) 0.7800(15) 0.8628(11) 0.026(4) Uiso 1 1 d G . .
C4 C 0.3134(11) 0.7725(14) 0.9076(11) 0.030(4) Uiso 1 1 d G . .
H4 H 0.3154 0.6829 0.9558 0.036 Uiso 1 1 calc R . .
C5 C 0.2743(10) 0.8988(17) 0.8802(12) 0.032(5) Uiso 1 1 d G . .
H5 H 0.2500 0.8938 0.9102 0.039 Uiso 1 1 calc R . .
C6 C 0.2713(10) 1.0327(16) 0.8081(12) 0.046(6) Uiso 1 1 d G . .
H6 H 0.2451 1.1172 0.7898 0.055 Uiso 1 1 calc R . .
C7 C 0.3076(11) 1.0402(15) 0.7633(11) 0.038(5) Uiso 1 1 d G . .
H7 H 0.3056 1.1298 0.7150 0.045 Uiso 1 1 calc R . .
C8 C 0.3468(10) 0.9139(17) 0.7906(12) 0.030(4) Uiso 1 1 d G . .
C9 C 0.433(3) 1.113(3) 0.778(3) 0.053(7) Uiso 1 1 d . . .
H9A H 0.4516 1.1043 0.8507 0.080 Uiso 1 1 calc R . .
H9B H 0.4108 1.2172 0.7647 0.080 Uiso 1 1 calc R . .
H9C H 0.4559 1.1272 0.7429 0.080 Uiso 1 1 calc R . .
C10 C 0.363(2) 0.956(3) 0.599(2) 0.035(5) Uiso 1 1 d . . .
H10A H 0.3417 0.8534 0.5685 0.052 Uiso 1 1 calc R . .
H10B H 0.3869 0.9742 0.5668 0.052 Uiso 1 1 calc R . .
H10C H 0.3423 1.0628 0.5911 0.052 Uiso 1 1 calc R . .
Br1 Br 0.3474(3) 0.5014(3) 0.6509(2) 0.077(5) Uani 1 1 d . . .
Br2 Br 0.5190(3) 0.8111(3) 0.9089(2) 0.083(5) Uani 1 1 d . . .
Ge1 Ge 0.4430(3) 0.6268(3) 0.7750(2) 0.083(5) Uani 1 1 d . . .
P1 P 0.4014(6) 0.6156(6) 0.9027(5) 0.064(11) Uani 1 1 d . . .
P2 P 0.3962(6) 0.9120(6) 0.7345(5) 0.070(11) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.164(15) 0.0361(11) 0.041(2) -0.0041(10) 0.049(5) -0.005(2)
Br2 0.167(17) 0.0364(11) 0.051(2) -0.0021(10) 0.047(6) 0.003(2)
Ge1 0.198(15) 0.0223(10) 0.041(2) -0.0020(9) 0.057(5) -0.003(2)
P1 0.14(3) 0.027(2) 0.034(4) 0.004(2) 0.042(12) 0.004(5)
P2 0.16(3) 0.018(2) 0.037(4) 0.005(2) 0.043(12) 0.008(5)

_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 P1 1.84(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 P1 1.78(4) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.3900 . ?
C3 C8 1.3900 . ?
C3 P1 1.82(2) . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 C6 1.3900 . ?
C5 H5 0.9300 . ?
C6 C7 1.3900 . ?
C6 H6 0.9300 . ?
C7 C8 1.3900 . ?
C7 H7 0.9300 . ?
C8 P2 1.84(2) . ?
C9 P2 1.78(4) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 P2 1.81(3) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
Br1 Ge1 2.789(10) . ?
Br2 Ge1 2.653(8) . ?
Ge1 P2 2.433(10) . ?
Ge1 P1 2.480(10) . ?

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
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 120.0 . . ?
C4 C3 P1 118.8(8) . . ?
C8 C3 P1 121.1(8) . . ?
C3 C4 C5 120.0 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C7 C6 C5 120.0 . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C8 120.0 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C3 120.0 . . ?
C7 C8 P2 123.1(8) . . ?
C3 C8 P2 116.9(8) . . ?
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 . . ?
P2 Ge1 P1 80.4(3) . . ?
P2 Ge1 Br2 87.7(4) . . ?
P1 Ge1 Br2 89.2(3) . . ?
P2 Ge1 Br1 79.3(4) . . ?
P1 Ge1 Br1 80.0(4) . . ?
Br2 Ge1 Br1 164.3(2) . . ?
C2 P1 C3 105.2(15) . . ?
C2 P1 C1 106.8(13) . . ?
C3 P1 C1 103.7(19) . . ?
C2 P1 Ge1 116.9(19) . . ?
C3 P1 Ge1 107.5(5) . . ?
C1 P1 Ge1 115.4(8) . . ?
C9 P2 C10 103.2(16) . . ?
C9 P2 C8 106.7(16) . . ?
C10 P2 C8 105(2) . . ?
C9 P2 Ge1 116(2) . . ?
C10 P2 Ge1 115.4(10) . . ?
C8 P2 Ge1 110.1(5) . . ?

_diffrn_measured_fraction_theta_max 0.289
_diffrn_reflns_theta_full        29.11
_diffrn_measured_fraction_theta_full 0.289
_refine_diff_density_max         1.676
_refine_diff_density_min         -1.419
_refine_diff_density_rms         0.421
_database_code_depnum_ccdc_archive 'CCDC 977915'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gebr2diphos4new


_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2012-08-24
# start Validation Reply Form
_vrf_PLAT029_gebr2diphos4new     
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.294     
RESPONSE: Data are collected using a diamond anvil cell which has a limited 
opening angle which restricts the data accessible to measure.
This resulting low completeness is typical of these studies.
;

_chemical_name_systematic        
;
 Dibromo(1,2-bis(dimethylphosphino)benzene-P,P')germanium(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H16 Br2 Ge P2'
_chemical_formula_sum            'C10 H16 Br2 Ge P2'
_chemical_formula_weight         430.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0028 0.0015 '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'
Br Br -0.1853 2.3459 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1952 1.7169 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0974 0.0893 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'

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'

_cell_length_a                   27.88(3)
_cell_length_b                   7.166(6)
_cell_length_c                   13.692(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.678(15)
_cell_angle_gamma                90.00
_cell_volume                     2542(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       2700000 # kpascals = 27kbar
_cell_measurement_reflns_used    611
_cell_measurement_theta_min      2.9
_cell_measurement_theta_max      29.2

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1664
_exptl_absorpt_coefficient_mu    8.219
_exptl_absorpt_correction_type   None
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293
_diffrn_ambient_pressure         2700000 #kpascals = 27kbar
_diffrn_measurement_specimen_support 'Diamond Anvil Cell'
_diffrn_radiation_wavelength     0.68890
_diffrn_radiation_type           synchrotron
_diffrn_source_type              'DLS beamline I19'
_diffrn_source                   synchrotron
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'


_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4594
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_sigmaI/netI    0.0606
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.86
_diffrn_reflns_theta_max         29.38
_reflns_number_total             1130
_reflns_number_gt                857
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;

_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1129
_refine_ls_number_parameters     74
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1132
_refine_ls_R_factor_gt           0.0830
_refine_ls_wR_factor_ref         0.3198
_refine_ls_wR_factor_gt          0.2495
_refine_ls_goodness_of_fit_ref   1.286
_refine_ls_restrained_S_all      1.286
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.364(2) 0.396(3) 0.9051(19) 0.037(5) Uiso 1 1 d . . .
H1A H 0.3443 0.3596 0.8341 0.055 Uiso 1 1 calc R . .
H1B H 0.3415 0.4216 0.9417 0.055 Uiso 1 1 calc R . .
H1C H 0.3872 0.2958 0.9399 0.055 Uiso 1 1 calc R . .
C2 C 0.4430(19) 0.667(2) 1.0389(16) 0.019(3) Uiso 1 1 d . . .
H2A H 0.4597 0.7845 1.0401 0.028 Uiso 1 1 calc R . .
H2B H 0.4686 0.5716 1.0671 0.028 Uiso 1 1 calc R . .
H2C H 0.4219 0.6755 1.0807 0.028 Uiso 1 1 calc R . .
C3 C 0.3514(9) 0.7736(14) 0.8656(10) 0.026(4) Uiso 1 1 d G . .
C4 C 0.3143(9) 0.7656(13) 0.9109(9) 0.025(4) Uiso 1 1 d G . .
H4 H 0.3161 0.6734 0.9600 0.030 Uiso 1 1 calc R . .
C5 C 0.2744(9) 0.8954(16) 0.8829(10) 0.035(4) Uiso 1 1 d G . .
H5 H 0.2496 0.8900 0.9132 0.042 Uiso 1 1 calc R . .
C6 C 0.2716(9) 1.0332(16) 0.8096(10) 0.039(5) Uiso 1 1 d G . .
H6 H 0.2450 1.1200 0.7908 0.047 Uiso 1 1 calc R . .
C7 C 0.3087(10) 1.0412(14) 0.7642(11) 0.041(5) Uiso 1 1 d G . .
H7 H 0.3069 1.1334 0.7151 0.050 Uiso 1 1 calc R . .
C8 C 0.3486(9) 0.9114(15) 0.7922(11) 0.029(4) Uiso 1 1 d G . .
C9 C 0.439(2) 1.123(2) 0.7809(18) 0.029(4) Uiso 1 1 d . . .
H9A H 0.4578 1.1133 0.8553 0.044 Uiso 1 1 calc R . .
H9B H 0.4191 1.2356 0.7658 0.044 Uiso 1 1 calc R . .
H9C H 0.4632 1.1263 0.7456 0.044 Uiso 1 1 calc R . .
C10 C 0.365(2) 0.962(3) 0.600(2) 0.035(5) Uiso 1 1 d . . .
H10A H 0.3431 0.8589 0.5660 0.053 Uiso 1 1 calc R . .
H10B H 0.3904 0.9805 0.5690 0.053 Uiso 1 1 calc R . .
H10C H 0.3442 1.0730 0.5901 0.053 Uiso 1 1 calc R . .
Br1 Br 0.3478(2) 0.5060(2) 0.6503(2) 0.080(4) Uani 1 1 d . . .
Br2 Br 0.5204(2) 0.8161(3) 0.9120(2) 0.076(4) Uani 1 1 d . . .
Ge1 Ge 0.4438(2) 0.6252(2) 0.77360(19) 0.060(4) Uani 1 1 d . . .
P1 P 0.4026(5) 0.6088(6) 0.9045(5) 0.050(8) Uani 1 1 d . . .
P2 P 0.3953(6) 0.9162(6) 0.7338(4) 0.082(9) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.186(14) 0.0283(10) 0.0430(19) -0.0046(8) 0.062(5) -0.0040(17)
Br2 0.164(13) 0.0299(11) 0.0451(19) -0.0015(8) 0.051(5) 0.0004(18)
Ge1 0.137(12) 0.0182(9) 0.0391(19) 0.0012(7) 0.048(4) 0.0023(16)
P1 0.10(3) 0.023(2) 0.033(4) 0.0007(18) 0.037(9) 0.008(4)
P2 0.21(3) 0.0165(19) 0.038(4) 0.0032(18) 0.063(10) 0.003(4)

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

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 P1 1.87(4) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 P1 1.82(3) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.3900 . ?
C3 C8 1.3900 . ?
C3 P1 1.78(2) . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 C6 1.3900 . ?
C5 H5 0.9300 . ?
C6 C7 1.3900 . ?
C6 H6 0.9300 . ?
C7 C8 1.3900 . ?
C7 H7 0.9300 . ?
C8 P2 1.76(2) . ?
C9 P2 1.88(4) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 P2 1.75(3) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
Br1 Ge1 2.721(8) . ?
Br2 Ge1 2.653(7) . ?
Ge1 P2 2.435(9) . ?
Ge1 P1 2.460(8) . ?

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
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 120.0 . . ?
C4 C3 P1 119.2(7) . . ?
C8 C3 P1 120.8(7) . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C7 C6 C5 120.0 . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C8 120.0 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C3 120.0 . . ?
C7 C8 P2 120.7(8) . . ?
C3 C8 P2 119.2(8) . . ?
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 . . ?
P2 Ge1 P1 80.5(3) . . ?
P2 Ge1 Br2 87.3(3) . . ?
P1 Ge1 Br2 88.5(3) . . ?
P2 Ge1 Br1 78.0(3) . . ?
P1 Ge1 Br1 79.7(3) . . ?
Br2 Ge1 Br1 162.5(2) . . ?
C3 P1 C2 106.2(11) . . ?
C3 P1 C1 98.4(18) . . ?
C2 P1 C1 108.9(11) . . ?
C3 P1 Ge1 106.8(4) . . ?
C2 P1 Ge1 116.6(14) . . ?
C1 P1 Ge1 117.7(7) . . ?
C10 P2 C8 109(2) . . ?
C10 P2 C9 102.3(13) . . ?
C8 P2 C9 110.9(11) . . ?
C10 P2 Ge1 114.3(9) . . ?
C8 P2 Ge1 108.9(5) . . ?
C9 P2 Ge1 111.2(15) . . ?

_diffrn_measured_fraction_theta_max 0.294
_diffrn_reflns_theta_full        29.38
_diffrn_measured_fraction_theta_full 0.294
_refine_diff_density_max         1.371
_refine_diff_density_min         -1.991
_refine_diff_density_rms         0.300
_database_code_depnum_ccdc_archive 'CCDC 977916'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gebr2diphos5

_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2013-01-16
# start Validation Reply Form
_vrf_PLAT029_gebr2diphos5        
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.272     
RESPONSE: Data are collected using a diamond anvil cell which has a limited 
opening angle which restricts the data accessible to measure.
This resulting low completeness is typical of these studies.
;
_chemical_name_systematic        
;
 Dibromo(1,2-bis(dimethylphosphino)benzene-P,P')germanium(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H16 Br2 Ge P2'
_chemical_formula_sum            'C10 H16 Br2 Ge P2'
_chemical_formula_weight         430.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0032 0.0015 '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'
Br Br -0.1750 2.4304 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.2186 1.7697 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0990 0.0908 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'

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'

_cell_length_a                   25.79(10)
_cell_length_b                   7.17(3)
_cell_length_c                   14.06(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.24(8)
_cell_angle_gamma                90.00
_cell_volume                     2598(17)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)

_cell_measurement_pressure       4100000 # kpascals = 41kbar
_cell_measurement_reflns_used    4667
_cell_measurement_theta_min      1.4
_cell_measurement_theta_max      28.6

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1664
_exptl_absorpt_coefficient_mu    8.041
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293
_diffrn_ambient_pressure         4100000 #kpascals = 41kbar
_diffrn_measurement_specimen_support 'Diamond Anvil Cell'
_diffrn_radiation_wavelength     0.68890
_diffrn_radiation_type           synchrotron
_diffrn_source_type              'DLS beamline I19'
_diffrn_source                   synchrotron
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4460
_diffrn_reflns_av_R_equivalents  0.1015
_diffrn_reflns_av_sigmaI/netI    0.1031
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.90
_diffrn_reflns_theta_max         29.80
_reflns_number_total             1012
_reflns_number_gt                593
_reflns_threshold_expression     I>2/sigma(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;

_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1583P)²+215.8169P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1012
_refine_ls_number_parameters     74
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1780
_refine_ls_R_factor_gt           0.1146
_refine_ls_wR_factor_ref         0.3481
_refine_ls_wR_factor_gt          0.2847
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.361(4) -0.442(5) 0.681(2) 0.054(9) Uiso 1 1 d . . .
H1A H 0.3399 -0.3366 0.6647 0.081 Uiso 1 1 calc R . .
H1B H 0.3402 -0.5521 0.6835 0.081 Uiso 1 1 calc R . .
H1C H 0.3866 -0.4585 0.6330 0.081 Uiso 1 1 calc R . .
C2 C 0.431(4) -0.616(4) 0.8186(19) 0.038(7) Uiso 1 1 d . . .
H2A H 0.4520 -0.6046 0.8759 0.056 Uiso 1 1 calc R . .
H2B H 0.4522 -0.6386 0.7657 0.056 Uiso 1 1 calc R . .
H2C H 0.4068 -0.7172 0.8249 0.056 Uiso 1 1 calc R . .
C3 C 0.3372(16) -0.411(3) 0.8867(11) 0.041(8) Uiso 1 1 d G . .
C4 C 0.2973(17) -0.541(3) 0.8787(11) 0.046(8) Uiso 1 1 d G . .
H4 H 0.2942 -0.6174 0.8252 0.055 Uiso 1 1 calc R . .
C5 C 0.2622(16) -0.558(3) 0.9508(14) 0.044(8) Uiso 1 1 d G . .
H5 H 0.2355 -0.6449 0.9454 0.053 Uiso 1 1 calc R . .
C6 C 0.2669(16) -0.444(3) 1.0307(12) 0.046(8) Uiso 1 1 d G . .
H6 H 0.2434 -0.4552 1.0789 0.055 Uiso 1 1 calc R . .
C7 C 0.3068(17) -0.314(3) 1.0387(10) 0.040(8) Uiso 1 1 d G . .
H7 H 0.3100 -0.2381 1.0922 0.048 Uiso 1 1 calc R . .
C8 C 0.3420(16) -0.298(3) 0.9666(12) 0.029(6) Uiso 1 1 d G . .
C9 C 0.442(3) -0.181(4) 1.0752(16) 0.030(6) Uiso 1 1 d . . .
H9A H 0.4687 -0.0895 1.0841 0.045 Uiso 1 1 calc R . .
H9B H 0.4568 -0.3007 1.0643 0.045 Uiso 1 1 calc R . .
H9C H 0.4215 -0.1858 1.1311 0.045 Uiso 1 1 calc R . .
C10 C 0.364(3) 0.104(4) 1.0050(18) 0.033(7) Uiso 1 1 d . . .
H10A H 0.3878 0.2073 1.0079 0.049 Uiso 1 1 calc R . .
H10B H 0.3487 0.0891 1.0656 0.049 Uiso 1 1 calc R . .
H10C H 0.3373 0.1283 0.9571 0.049 Uiso 1 1 calc R . .
P1 P 0.3951(10) -0.4031(9) 0.7987(5) 0.077(15) Uani 1 1 d . . .
P2 P 0.4003(9) -0.1168(10) 0.9737(5) 0.040(15) Uani 1 1 d . . .
Ge1 Ge 0.4400(4) -0.1071(4) 0.8152(2) 0.064(6) Uani 1 1 d . . .
Br1 Br 0.5188(4) -0.3034(4) 0.8951(2) 0.079(7) Uani 1 1 d . . .
Br2 Br 0.3318(4) 0.0076(4) 0.76043(19) 0.065(7) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.17(5) 0.019(3) 0.038(3) 0.002(3) -0.005(8) -0.017(8)
P2 0.06(5) 0.026(3) 0.033(3) 0.001(2) -0.010(7) 0.014(7)
Ge1 0.13(2) 0.0184(13) 0.0405(16) -0.0009(10) 0.010(3) 0.000(3)
Br1 0.15(2) 0.0331(16) 0.0552(18) -0.0030(12) 0.007(4) 0.004(3)
Br2 0.12(2) 0.0311(15) 0.0394(15) -0.0011(10) 0.001(3) 0.004(3)

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

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 P1 1.86(5) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 P1 1.80(5) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.3900 . ?
C3 C8 1.3900 . ?
C3 P1 1.98(4) . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 C6 1.3900 . ?
C5 H5 0.9300 . ?
C6 C7 1.3900 . ?
C6 H6 0.9300 . ?
C7 C8 1.3900 . ?
C7 H7 0.9300 . ?
C8 P2 1.99(4) . ?
C9 P2 1.81(5) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 P2 1.90(5) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
P1 Ge1 2.425(16) . ?
P2 Ge1 2.490(15) . ?
Ge1 Br1 2.682(13) . ?

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
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 120.0 . . ?
C4 C3 P1 123.0(12) . . ?
C8 C3 P1 116.4(13) . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 120.0 . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C8 C7 C6 120.0 . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C3 120.0 . . ?
C7 C8 P2 122.2(11) . . ?
C3 C8 P2 117.8(11) . . ?
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 . . ?
C2 P1 C1 103(2) . . ?
C2 P1 C3 106(2) . . ?
C1 P1 C3 102(3) . . ?
C2 P1 Ge1 119(3) . . ?
C1 P1 Ge1 114.9(15) . . ?
C3 P1 Ge1 109.6(7) . . ?
C9 P2 C10 108.1(18) . . ?
C9 P2 C8 107.3(19) . . ?
C10 P2 C8 100(3) . . ?
C9 P2 Ge1 118(2) . . ?
C10 P2 Ge1 114.0(10) . . ?
C8 P2 Ge1 108.1(7) . . ?
P1 Ge1 P2 81.3(5) . . ?
P1 Ge1 Br1 86.1(6) . . ?
P2 Ge1 Br1 86.7(5) . . ?

_diffrn_measured_fraction_theta_max 0.272
_diffrn_reflns_theta_full        29.80
_diffrn_measured_fraction_theta_full 0.272
_refine_diff_density_max         0.939
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.247
_database_code_depnum_ccdc_archive 'CCDC 977917'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gebr2diphos6

_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2013-01-24

# start Validation Reply Form
_vrf_PLAT029_gebr2diphos6        
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.291      
RESPONSE: Data are collected using a diamond anvil cell which has a limited 
opening angle which restricts the data accessible to measure.
This resulting low completeness is typical of these studies.
;
_chemical_name_systematic        
;
 Dibromo(1,2-bis(dimethylphosphino)benzene-P,P')germanium(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H16 Br2 Ge P2'
_chemical_formula_sum            'C10 H16 Br2 Ge P2'
_chemical_formula_weight         430.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0032 0.0015 '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'
Br Br -0.1750 2.4304 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.2186 1.7697 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0990 0.0908 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'

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'

_cell_length_a                   24.773(10)
_cell_length_b                   6.98(3)
_cell_length_c                   13.67(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.25(11)
_cell_angle_gamma                90.00
_cell_volume                     2362(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       5400000 # kpascals = 54kbar
_cell_measurement_reflns_used    410
_cell_measurement_theta_min      2.9
_cell_measurement_theta_max      28.4

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1664
_exptl_absorpt_coefficient_mu    8.845
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.582
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293
_diffrn_ambient_pressure         5400000 #kpascals = 54kbar
_diffrn_measurement_specimen_support 'Diamond Anvil Cell'
_diffrn_radiation_wavelength     0.68890
_diffrn_radiation_type           synchrotron
_diffrn_source_type              'DLS beamline I19'
_diffrn_source                   synchrotron
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'


_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4347
_diffrn_reflns_av_R_equivalents  0.0979
_diffrn_reflns_av_sigmaI/netI    0.0916
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.89
_diffrn_reflns_theta_max         28.65
_reflns_number_total             970
_reflns_number_gt                649
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;

_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0449P)²+432.9641P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         970
_refine_ls_number_parameters     64
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1576
_refine_ls_R_factor_gt           0.1077
_refine_ls_wR_factor_ref         0.2628
_refine_ls_wR_factor_gt          0.2252
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.359(3) -0.447(4) 0.6829(19) 0.038(7) Uiso 1 1 d . . .
H1A H 0.3372 -0.3381 0.6665 0.056 Uiso 1 1 calc R . .
H1B H 0.3367 -0.5583 0.6890 0.056 Uiso 1 1 calc R . .
H1C H 0.3843 -0.4687 0.6323 0.056 Uiso 1 1 calc R . .
C2 C 0.433(3) -0.611(4) 0.8173(19) 0.035(7) Uiso 1 1 d . . .
H2A H 0.4546 -0.5976 0.8765 0.052 Uiso 1 1 calc R . .
H2B H 0.4556 -0.6318 0.7632 0.052 Uiso 1 1 calc R . .
H2C H 0.4086 -0.7171 0.8233 0.052 Uiso 1 1 calc R . .
C3 C 0.3405(16) -0.412(3) 0.8830(12) 0.044(8) Uiso 1 1 d G . .
C4 C 0.2986(16) -0.544(3) 0.8736(10) 0.047(9) Uiso 1 1 d G . .
H4 H 0.2952 -0.6206 0.8179 0.056 Uiso 1 1 calc R . .
C5 C 0.2620(15) -0.563(3) 0.9474(12) 0.031(7) Uiso 1 1 d G . .
H5 H 0.2340 -0.6514 0.9410 0.038 Uiso 1 1 calc R . .
C6 C 0.2671(15) -0.449(3) 1.0306(11) 0.037(7) Uiso 1 1 d G . .
H6 H 0.2425 -0.4613 1.0800 0.044 Uiso 1 1 calc R . .
C7 C 0.3089(16) -0.317(2) 1.0401(10) 0.030(6) Uiso 1 1 d G . .
H7 H 0.3123 -0.2404 1.0958 0.035 Uiso 1 1 calc R . .
C8 C 0.3456(15) -0.298(3) 0.9663(13) 0.031(6) Uiso 1 1 d G . .
C9 C 0.445(3) -0.175(4) 1.0832(18) 0.034(7) Uiso 1 1 d . . .
H9A H 0.4725 -0.0787 1.0906 0.050 Uiso 1 1 calc R . .
H9B H 0.4618 -0.2977 1.0735 0.050 Uiso 1 1 calc R . .
H9C H 0.4244 -0.1795 1.1410 0.050 Uiso 1 1 calc R . .
C10 C 0.374(3) 0.106(3) 1.0063(16) 0.025(6) Uiso 1 1 d . . .
H10A H 0.4024 0.1988 1.0068 0.037 Uiso 1 1 calc R . .
H10B H 0.3595 0.0978 1.0704 0.037 Uiso 1 1 calc R . .
H10C H 0.3457 0.1441 0.9600 0.037 Uiso 1 1 calc R . .
P1 P 0.3959(8) -0.4047(9) 0.7975(4) 0.0245(15) Uiso 1 1 d . . .
P2 P 0.3989(8) -0.1162(9) 0.9733(4) 0.0251(16) Uiso 1 1 d . . .
Ge1 Ge 0.4409(4) -0.1059(4) 0.81389(19) 0.066(6) Uani 1 1 d . . .
Br1 Br 0.5193(4) -0.3048(4) 0.8959(2) 0.079(6) Uani 1 1 d . . .
Br2 Br 0.3305(4) 0.0065(4) 0.75949(18) 0.076(6) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ge1 0.150(18) 0.0148(12) 0.0326(14) 0.0007(10) 0.009(3) -0.009(3)
Br1 0.17(2) 0.0211(13) 0.0463(16) 0.0003(11) 0.004(3) 0.003(3)
Br2 0.173(18) 0.0227(12) 0.0321(13) 0.0015(10) 0.002(3) -0.002(3)

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

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 P1 1.80(5) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 P1 1.72(5) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.3900 . ?
C3 C8 1.3900 . ?
C3 P1 1.84(3) . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 C6 1.3900 . ?
C5 H5 0.9300 . ?
C6 C7 1.3900 . ?
C6 H6 0.9300 . ?
C7 C8 1.3900 . ?
C7 H7 0.9300 . ?
C8 P2 1.83(3) . ?
C9 P2 1.90(5) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 P2 1.74(4) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
P1 Ge1 2.371(14) . ?
P2 Ge1 2.452(14) . ?
Ge1 Br1 2.605(11) . ?

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
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 120.0 . . ?
C4 C3 P1 122.1(12) . . ?
C8 C3 P1 117.3(13) . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C7 C6 C5 120.0 . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C8 C7 C6 120.0 . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C3 120.0 . . ?
C7 C8 P2 121.1(12) . . ?
C3 C8 P2 118.8(11) . . ?
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 . . ?
C2 P1 C1 104(2) . . ?
C2 P1 C3 106(2) . . ?
C1 P1 C3 101(3) . . ?
C2 P1 Ge1 118(2) . . ?
C1 P1 Ge1 116.5(12) . . ?
C3 P1 Ge1 108.9(7) . . ?
C10 P2 C8 112(3) . . ?
C10 P2 C9 101.5(17) . . ?
C8 P2 C9 107.5(17) . . ?
C10 P2 Ge1 111.9(11) . . ?
C8 P2 Ge1 107.7(7) . . ?
C9 P2 Ge1 116(2) . . ?
P1 Ge1 P2 81.0(4) . . ?
P1 Ge1 Br1 84.9(5) . . ?
P2 Ge1 Br1 86.4(4) . . ?

_diffrn_measured_fraction_theta_max 0.291
_diffrn_reflns_theta_full        28.65
_diffrn_measured_fraction_theta_full 0.291
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.929
_refine_diff_density_rms         0.228
_database_code_depnum_ccdc_archive 'CCDC 977918'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gebr2diphos7

_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2012-08-26

# start Validation Reply Form
_vrf_PLAT029_gebr2diphos7        
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.286      
RESPONSE: Data are collected using a diamond anvil cell which has a limited 
opening angle which restricts the data accessible to measure.
This resulting low completeness is typical of these studies.
;

_chemical_name_systematic        
;
 Dibromo(1,2-bis(dimethylphosphino)benzene-P,P')germanium(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H16 Br2 Ge P2'
_chemical_formula_sum            'C10 H16 Br2 Ge P2'
_chemical_formula_weight         430.58

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'

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'

_cell_length_a                   24.73(6)
_cell_length_b                   6.956(13)
_cell_length_c                   13.63(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.59(6)
_cell_angle_gamma                90.00
_cell_volume                     2342(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       6300000 # kpascals = 63kbar
_cell_measurement_reflns_used    710
_cell_measurement_theta_min      1.4
_cell_measurement_theta_max      28.6

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1664
_exptl_absorpt_coefficient_mu    8.921
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293
_diffrn_ambient_pressure         6300000 #kpascals = 63kbar
_diffrn_measurement_specimen_support 'Diamond Anvil Cell'
_diffrn_radiation_wavelength     0.68890
_diffrn_radiation_type           ?
_diffrn_source_type              'DLS beamline I19'
_diffrn_source                   synchrotron
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'


_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4063
_diffrn_reflns_av_R_equivalents  0.0899
_diffrn_reflns_av_sigmaI/netI    0.0926
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         29.57
_reflns_number_total             942
_reflns_number_gt                610
_reflns_threshold_expression     I>2/sigma(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;

_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0449P)²+432.9641P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         942
_refine_ls_number_parameters     74
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1659
_refine_ls_R_factor_gt           0.1072
_refine_ls_wR_factor_ref         0.2808
_refine_ls_wR_factor_gt          0.2340
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_restrained_S_all      1.118
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.359(4) -0.452(5) 0.682(2) 0.046(10) Uiso 1 1 d . . .
H1A H 0.3370 -0.3432 0.6645 0.069 Uiso 1 1 calc R . .
H1B H 0.3371 -0.5634 0.6891 0.069 Uiso 1 1 calc R . .
H1C H 0.3845 -0.4741 0.6316 0.069 Uiso 1 1 calc R . .
C2 C 0.434(4) -0.616(5) 0.818(2) 0.043(9) Uiso 1 1 d . . .
H2A H 0.4564 -0.6031 0.8774 0.065 Uiso 1 1 calc R . .
H2B H 0.4572 -0.6376 0.7638 0.065 Uiso 1 1 calc R . .
H2C H 0.4102 -0.7231 0.8238 0.065 Uiso 1 1 calc R . .
C3 C 0.3417(17) -0.409(3) 0.8831(13) 0.033(7) Uiso 1 1 d G . .
C4 C 0.2997(17) -0.541(3) 0.8715(11) 0.047(10) Uiso 1 1 d G . .
H4 H 0.2963 -0.6153 0.8148 0.056 Uiso 1 1 calc R . .
C5 C 0.2629(16) -0.563(3) 0.9448(13) 0.027(7) Uiso 1 1 d G . .
H5 H 0.2348 -0.6513 0.9370 0.033 Uiso 1 1 calc R . .
C6 C 0.2679(16) -0.452(3) 1.0296(12) 0.031(7) Uiso 1 1 d G . .
H6 H 0.2433 -0.4665 1.0786 0.038 Uiso 1 1 calc R . .
C7 C 0.3099(17) -0.320(3) 1.0412(10) 0.031(7) Uiso 1 1 d G . .
H7 H 0.3133 -0.2458 1.0980 0.037 Uiso 1 1 calc R . .
C8 C 0.3467(16) -0.298(3) 0.9680(13) 0.026(6) Uiso 1 1 d G . .
C9 C 0.442(3) -0.179(4) 1.0826(19) 0.030(7) Uiso 1 1 d . . .
H9A H 0.4703 -0.0848 1.0923 0.045 Uiso 1 1 calc R . .
H9B H 0.4580 -0.3031 1.0732 0.045 Uiso 1 1 calc R . .
H9C H 0.4205 -0.1823 1.1393 0.045 Uiso 1 1 calc R . .
C10 C 0.375(3) 0.107(4) 1.006(2) 0.029(7) Uiso 1 1 d . . .
H10A H 0.4034 0.1995 1.0061 0.044 Uiso 1 1 calc R . .
H10B H 0.3604 0.0995 1.0699 0.044 Uiso 1 1 calc R . .
H10C H 0.3464 0.1457 0.9590 0.044 Uiso 1 1 calc R . .
P1 P 0.3964(10) -0.4034(10) 0.7971(5) 0.065(16) Uani 1 1 d . . .
P2 P 0.3990(9) -0.1148(10) 0.9731(5) 0.033(14) Uani 1 1 d . . .
Ge1 Ge 0.4410(4) -0.1045(4) 0.8133(2) 0.054(6) Uani 1 1 d . . .
Br1 Br 0.5189(4) -0.3061(4) 0.8965(2) 0.061(7) Uani 1 1 d . . .
Br2 Br 0.3304(4) 0.0053(4) 0.7590(2) 0.056(6) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.14(5) 0.020(3) 0.032(4) -0.005(3) 0.017(8) -0.013(8)
P2 0.06(4) 0.019(3) 0.024(3) 0.001(2) 0.000(7) 0.004(7)
Ge1 0.11(2) 0.0196(14) 0.0328(16) -0.0011(11) 0.009(3) -0.004(3)
Br1 0.11(2) 0.0270(15) 0.0464(18) -0.0002(12) 0.004(4) 0.008(3)
Br2 0.11(2) 0.0270(14) 0.0317(14) 0.0030(11) 0.003(3) 0.002(3)

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

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 P1 1.81(6) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 P1 1.77(6) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.3900 . ?
C3 C8 1.3900 . ?
C3 P1 1.83(3) . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 C6 1.3900 . ?
C5 H5 0.9300 . ?
C6 C7 1.3900 . ?
C6 H6 0.9300 . ?
C7 C8 1.3900 . ?
C7 H7 0.9300 . ?
C8 P2 1.82(3) . ?
C9 P2 1.85(5) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 P2 1.72(4) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
P1 Ge1 2.359(15) . ?
P2 Ge1 2.455(13) . ?
Ge1 Br1 2.601(12) . ?

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
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 120.0 . . ?
C4 C3 P1 120.7(13) . . ?
C8 C3 P1 118.6(14) . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C7 C6 C5 120.0 . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C8 120.0 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C3 120.0 . . ?
C7 C8 P2 122.5(12) . . ?
C3 C8 P2 117.3(11) . . ?
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 . . ?
C2 P1 C1 103(2) . . ?
C2 P1 C3 106(2) . . ?
C1 P1 C3 101(3) . . ?
C2 P1 Ge1 119(3) . . ?
C1 P1 Ge1 117.4(14) . . ?
C3 P1 Ge1 108.3(8) . . ?
C10 P2 C8 112(3) . . ?
C10 P2 C9 102(2) . . ?
C8 P2 C9 104.2(19) . . ?
C10 P2 Ge1 111.7(13) . . ?
C8 P2 Ge1 108.4(7) . . ?
C9 P2 Ge1 118(2) . . ?
P1 Ge1 P2 81.0(4) . . ?
P1 Ge1 Br1 84.2(6) . . ?
P2 Ge1 Br1 86.1(5) . . ?

_diffrn_measured_fraction_theta_max 0.286
_diffrn_reflns_theta_full        29.57
_diffrn_measured_fraction_theta_full 0.286
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.983
_refine_diff_density_rms         0.258
_database_code_depnum_ccdc_archive 'CCDC 977919'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gebr2diphos8

_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2012-08-26

# start Validation Reply Form
_vrf_PLAT029_gebr2diphos8        
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.274     
RESPONSE: Data are collected using a diamond anvil cell which has a limited 
opening angle which restricts the data accessible to measure.
This resulting low completeness is typical of these studies.
;
_chemical_name_systematic        
;
 Dibromo(1,2-bis(dimethylphosphino)benzene-P,P')germanium(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H16 Br2 Ge P2'
_chemical_formula_sum            'C10 H16 Br2 Ge P2'
_chemical_formula_weight         430.58


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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'

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'

_cell_length_a                   24.56(16)
_cell_length_b                   6.89(4)
_cell_length_c                   13.52(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.65(18)
_cell_angle_gamma                90.00
_cell_volume                     2286(24)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       8000000 # kpascals = 80kbar
_cell_measurement_reflns_used    677
_cell_measurement_theta_min      1.5
_cell_measurement_theta_max      35.7

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1664
_exptl_absorpt_coefficient_mu    9.143
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293
_diffrn_ambient_pressure         100000 #kpascals = 1kbar
_diffrn_measurement_specimen_support 'Diamond Anvil Cell'
_diffrn_radiation_wavelength     0.68890
_diffrn_radiation_type           ?
_diffrn_source_type              'DLS beamline I19'
_diffrn_source                   synchrotron
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'


_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3325
_diffrn_reflns_av_R_equivalents  0.0930
_diffrn_reflns_av_sigmaI/netI    0.1133
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         29.63
_reflns_number_total             887
_reflns_number_gt                558
_reflns_threshold_expression     I>2/sigma(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0231P)²+451.2141P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         887
_refine_ls_number_parameters     74
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1591
_refine_ls_R_factor_gt           0.1030
_refine_ls_wR_factor_ref         0.2652
_refine_ls_wR_factor_gt          0.2284
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.371(4) 0.392(4) 0.504(2) 0.033(7) Uiso 1 1 d . . .
H1A H 0.3984 0.2931 0.5075 0.049 Uiso 1 1 calc R . .
H1B H 0.3434 0.3588 0.4544 0.049 Uiso 1 1 calc R . .
H1C H 0.3548 0.4038 0.5671 0.049 Uiso 1 1 calc R . .
C2 C 0.445(3) 0.680(3) 0.5816(15) 0.013(5) Uiso 1 1 d . . .
H2A H 0.4608 0.8039 0.5703 0.019 Uiso 1 1 calc R . .
H2B H 0.4728 0.5841 0.5915 0.019 Uiso 1 1 calc R . .
H2C H 0.4234 0.6858 0.6393 0.019 Uiso 1 1 calc R . .
C3 C 0.3458(17) 0.793(3) 0.4658(13) 0.026(7) Uiso 1 1 d G . .
C4 C 0.3083(18) 0.813(3) 0.5392(11) 0.034(8) Uiso 1 1 d G . .
H4 H 0.3109 0.7339 0.5950 0.041 Uiso 1 1 calc R . .
C5 C 0.2670(17) 0.950(3) 0.5291(13) 0.030(7) Uiso 1 1 d G . .
H5 H 0.2420 0.9633 0.5782 0.036 Uiso 1 1 calc R . .
C6 C 0.2632(17) 1.068(3) 0.4457(15) 0.037(8) Uiso 1 1 d G . .
H6 H 0.2356 1.1603 0.4390 0.045 Uiso 1 1 calc R . .
C7 C 0.3007(18) 1.049(3) 0.3723(11) 0.034(8) Uiso 1 1 d G . .
H7 H 0.2981 1.1278 0.3165 0.041 Uiso 1 1 calc R . .
C8 C 0.3419(17) 0.911(3) 0.3824(12) 0.028(7) Uiso 1 1 d G . .
C9 C 0.434(4) 1.131(5) 0.319(2) 0.040(9) Uiso 1 1 d . . .
H9A H 0.4624 1.1403 0.2733 0.060 Uiso 1 1 calc R . .
H9B H 0.4487 1.1301 0.3853 0.060 Uiso 1 1 calc R . .
H9C H 0.4094 1.2395 0.3096 0.060 Uiso 1 1 calc R . .
C10 C 0.361(4) 0.959(5) 0.179(2) 0.039(8) Uiso 1 1 d . . .
H10A H 0.3870 0.9559 0.1274 0.058 Uiso 1 1 calc R . .
H10B H 0.3453 1.0857 0.1816 0.058 Uiso 1 1 calc R . .
H10C H 0.3331 0.8647 0.1644 0.058 Uiso 1 1 calc R . .
P1 P 0.4004(10) 0.6120(10) 0.4737(5) 0.031(15) Uani 1 1 d . . .
P2 P 0.3951(10) 0.9031(9) 0.2948(6) 0.051(16) Uani 1 1 d . . .
Ge1 Ge 0.4423(4) 0.6020(4) 0.3120(2) 0.061(7) Uani 1 1 d . . .
Br1 Br 0.5193(4) 0.8072(4) 0.3983(2) 0.077(7) Uani 1 1 d . . .
Br2 Br 0.3304(4) 0.4957(4) 0.2583(2) 0.075(7) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.05(5) 0.020(3) 0.027(3) 0.003(2) 0.018(7) 0.001(7)
P2 0.10(5) 0.012(3) 0.039(4) 0.000(3) 0.013(9) 0.009(7)
Ge1 0.14(2) 0.0163(13) 0.0292(15) -0.0008(10) 0.010(3) 0.003(3)
Br1 0.17(2) 0.0229(13) 0.0432(17) -0.0004(12) 0.008(4) 0.000(3)
Br2 0.17(2) 0.0220(12) 0.0296(14) 0.0004(10) 0.004(3) 0.004(3)

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

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 P1 1.73(5) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 P1 1.84(5) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.3900 . ?
C3 C8 1.3900 . ?
C3 P1 1.83(4) . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 C6 1.3900 . ?
C5 H5 0.9300 . ?
C6 C7 1.3900 . ?
C6 H6 0.9300 . ?
C7 C8 1.3900 . ?
C7 H7 0.9300 . ?
C8 P2 1.80(4) . ?
C9 P2 1.85(6) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 P2 1.78(5) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
P1 Ge1 2.458(18) . ?
P2 Ge1 2.383(18) . ?
Ge1 Br1 2.596(16) . ?

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
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 120.0 . . ?
C4 C3 P1 122.1(13) . . ?
C8 C3 P1 117.9(12) . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 120.0 . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C6 C7 C8 120.0 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C3 120.0 . . ?
C7 C8 P2 120.3(13) . . ?
C3 C8 P2 119.4(14) . . ?
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 . . ?
C1 P1 C3 107(3) . . ?
C1 P1 C2 105.7(19) . . ?
C3 P1 C2 106.1(17) . . ?
C1 P1 Ge1 112.5(13) . . ?
C3 P1 Ge1 107.6(8) . . ?
C2 P1 Ge1 117(2) . . ?
C10 P2 C8 104(3) . . ?
C10 P2 C9 101(2) . . ?
C8 P2 C9 104(2) . . ?
C10 P2 Ge1 118.6(14) . . ?
C8 P2 Ge1 109.1(8) . . ?
C9 P2 Ge1 119(3) . . ?
P2 Ge1 P1 80.9(5) . . ?
P2 Ge1 Br1 84.9(7) . . ?
P1 Ge1 Br1 84.9(6) . . ?

_diffrn_measured_fraction_theta_max 0.274
_diffrn_reflns_theta_full        29.63
_diffrn_measured_fraction_theta_full 0.274
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.233
_database_code_depnum_ccdc_archive 'CCDC 977920'
