Supplementary Material (ESI) for Dalton Tranactions
This journal is (c) The Royal Society of Chemistry 2003


data_global

_journal_coden_Cambridge         222

loop_
_publ_author_name
'A. Downs'
'Robert A.Coxall'
'T. M. Greene'
'Lorna Kettle'
'S. Parsons'
'David W. H. Rankin'
'Heather E. Robertson'
'Christina Y. Tang'
'Andrew R. Turner'

_publ_contact_author_name        'Prof A Downs'
_publ_contact_author_address     
;
Inorganic Chemistry Laboratory
University of Oxford
South Parks Road
Oxford
OX1 3QR
UNITED KINGDOM
;

_publ_contact_author_email       TONY.DOWNS@CHEM.OX.AC.UK

_publ_requested_journal          'Dalton Transactions'

_publ_section_title              
;
Molecular structure of trimethylphosphine-gallane,
Me3PGaH3: gas-phase electron diffraction, single-crystal X-ray
diffraction, and quantum chemical studies
;

data_ctga01
_database_code_CSD               212672

#Please see end of cif for Checkcif output

_audit_creation_date             02-15-09
_audit_creation_method           CRYSTALS_ver_12-03-99

_chemical_name_systematic        # IUPAC name, in full
;
?
;

_chemical_melting_point          'not measured'

_refine_ls_matrix_type           full
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    'Restrained refall, with common Uiso'

#************************************************************
# General computing
#=============================================================
_computing_structure_refinement  
;
CRYSTALS (Watkin et al 2001)
;
_computing_publication_material  
;
CRYSTALS (Watkin et al 2001)
;
_computing_molecular_graphics    
;
CAMERON (Watkin et al 1996)
;
#=============================================================

_cell_length_a                   5.8848(15)
_cell_angle_alpha                90
_cell_length_b                   9.212(2)
_cell_angle_beta                 113.879(4)
_cell_length_c                   7.0781(18)
_cell_angle_gamma                90
_cell_volume                     350.87(16)

_symmetry_cell_setting           'Monoclinic '
_symmetry_space_group_name_H-M   'P 21/m '
_symmetry_space_group_name_Hall  '-P 2yb'

loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z
x,-y+1/2,z

# choose from: rm (reference molecule of
# known chirality), ad (anomolous
# dispersion - ie. Flack param), rmad
# (both rm and ad), syn (known from
# synthetic pathway), unk (unknown)
# or . (not applicable).

_chemical_absolute_configuration .

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'C   ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 International_Tables_Vol_IV_Table_2.2B
'H   ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997
0.0030 International_Tables_Vol_IV_Table_2.2B
'P   ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 International_Tables_Vol_IV_Table_2.2B
'Ga  ' 0.1630 1.6090 15.2354 3.0669 6.7006 0.2412 4.3591 10.7805 2.9623 61.4135
1.7189 International_Tables_Vol_IV_Table_2.2B

_cell_formula_units_Z            2
_chemical_formula_sum            ' C3 H12 Ga1 P1 '
_chemical_formula_moiety         Me3P-GaH3
_chemical_compound_source        
;
?
;
_chemical_formula_weight         148.82

_cell_measurement_reflns_used    1874
_cell_measurement_theta_min      3
_cell_measurement_theta_max      29
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_max          0.07

_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_meas      'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000             152.000
_exptl_absorpt_coefficient_mu    4.020
# Sheldrick geometric definitions 0.75 0.55

_diffrn_measurement_device_type  
;
Bruker SMART
;
_diffrn_radiation_monochromator  graphite
_computing_data_collection       
;
SMART (Siemens, 1993)
;
_computing_data_reduction        
;
SAINT (Siemens ,1995)
;
_computing_cell_refinement       
;
SAINT (Siemens ,1995)
;
_computing_structure_solution    
;
SHELXS 86 (Sheldrick, 1986)
;
_diffrn_measurement_method       '\f & \w scans'
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS
;
_exptl_absorpt_correction_T_min  0.421
_exptl_absorpt_correction_T_max  0.550

#T min and max before scaling by 0.55 (Platon, Checkcif):
#_exptl_absorpt_correction_T_min   0.765
#_exptl_absorpt_correction_T_max   1.000

_diffrn_standards_interval_time  0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0.00

_diffrn_ambient_temperature      150
_diffrn_reflns_number            918
_reflns_number_total             918
_diffrn_reflns_av_R_equivalents  0.02
# Number of reflections with Friedels Law is 918
# Number of reflections without Friedels Law is 0
# Theoretical number of reflections is about 933

_diffrn_reflns_theta_min         3.147
_diffrn_reflns_theta_max         28.997
_diffrn_measured_fraction_theta_max 0.934

_diffrn_reflns_theta_full        27.692
_diffrn_measured_fraction_theta_full 0.998

_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       9
_reflns_limit_h_min              -7
_reflns_limit_h_max              7
_reflns_limit_k_min              0
_reflns_limit_k_max              12
_reflns_limit_l_min              0
_reflns_limit_l_max              9

_refine_diff_density_min         -0.33
_refine_diff_density_max         0.74

_refine_ls_number_reflns         914
_refine_ls_number_parameters     50

#_refine_ls_R_factor_ref 0.0239
_refine_ls_wR_factor_ref         0.0575
_refine_ls_goodness_of_fit_ref   1.0359

#_reflns_number_all 918
_refine_ls_R_factor_all          0.0242
_refine_ls_wR_factor_all         0.0589

# No actual I/u(I) cutoff was used for refinement. The
# threshold below is used for "_gt" information ONLY:
_reflns_threshold_expression     I>2.00u(I)
_reflns_number_gt                845
_refine_ls_R_factor_gt           0.0226
_refine_ls_wR_factor_gt          0.0574

_refine_ls_shift/su_max          0.0003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method = SHELXL 97 (Sheldrick, 1997)
W = q / [Sigma^2(F*)+(P(1)p)^2+P(2)p+P(4)+P(5)Sin(theta) ]

0.303E-01 0.850E-01 0.00 0.00 0.00 0.333
;
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073

## -------------------REFERENCES ----------------------##
## Insert your own references - in alphabetic order
_publ_section_references         
;

Siemens Industrial Automation, Inc (1993)
SMART: Area-Detector Software Package; Madison, WI.

Siemens Industrial Automation, Inc (1995).
SAINT: Area-Detector Integration Software.; Madison, WI.

Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.

Sheldrick, G.M. (1986). SHELXS86. Program for the solution of
crystal structures. Univ. of Gottingen, Federal Republic of Germany.

Sheldrick, G.M. (1997). SHELXL-97. Program for the refinement of
crystal structures. Univ. of Gottingen, Federal Republic of Germany.

Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper
R.I. (2001) CRYSTALS
Issue 11. Chemical Crystallography Laboratory, OXFORD, UK.

Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical
Crystallography Laboratory, OXFORD, UK.
;

# Uequiv = arithmetic mean of Ui
# i.e. Ueqiv = (U1+U2+U3)/3

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_occupancy
_atom_site_adp_type
_atom_site_attached_hydrogens
Ga1 Ga 0.38232(5) 0.2500 0.37069(4) 0.0285 1.0000 Uani .
P1 P 0.37713(11) 0.2500 0.70598(9) 0.0218 1.0000 Uani .
C1 C 0.2237(4) 0.0960(2) 0.7569(3) 0.0308 1.0000 Uani .
C2 C 0.6828(5) 0.2500 0.9100(4) 0.0323 1.0000 Uani .
H1 H 0.655(3) 0.2500 0.403(5) 0.027(5) 1.0000 Uiso .
H2 H 0.246(4) 0.110(2) 0.264(3) 0.027(5) 1.0000 Uiso .
H11 H 0.236(5) 0.098(3) 0.892(3) 0.042(4) 1.0000 Uiso .
H12 H 0.300(4) 0.014(2) 0.744(4) 0.042(4) 1.0000 Uiso .
H13 H 0.059(3) 0.097(3) 0.667(4) 0.042(4) 1.0000 Uiso .
H21 H 0.681(7) 0.2500 1.039(4) 0.040(6) 1.0000 Uiso .
H22 H 0.766(5) 0.332(2) 0.903(4) 0.040(6) 1.0000 Uiso .

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
Ga1 0.03207(17) 0.03642(19) 0.02066(15) 0.0000 0.01456(12) 0.0000
P1 0.0245(3) 0.0245(3) 0.0188(3) 0.0000 0.0114(2) 0.0000
C1 0.0377(9) 0.027(1) 0.0329(8) 0.0005(8) 0.0195(8) -0.0026(8)
C2 0.0268(12) 0.0432(17) 0.0262(11) 0.0000 0.010(1) 0.0000
_refine_ls_extinction_method     None

loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ga1 . P1 . 2.3857(6) yes
Ga1 . H1 . 1.526(17) no
Ga1 . H2 . 1.547(15) no
P1 . C1 . 1.795(2) yes
P1 . C2 . 1.794(3) yes
C1 . H11 . 0.928(16) no
C1 . H12 . 0.904(17) no
C1 . H13 . 0.920(16) no
C2 . H21 . 0.916(18) no
C2 . H22 . 0.913(16) no

loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
P1 . Ga1 . H1 . 106.8(13) no
P1 . Ga1 . H2 . 105.8(8) no
H1 . Ga1 . H2 . 112.2(10) no
P1 . Ga1 . H2 4_555 105.8(8) no
H1 . Ga1 . H2 4_555 112.2(10) no
H2 . Ga1 . H2 4_555 113.3(17) no
Ga1 . P1 . C1 . 114.20(7) yes
Ga1 . P1 . C1 4_555 114.20(7) yes
C1 . P1 . C1 4_555 104.43(13) yes
Ga1 . P1 . C2 . 112.84(9) yes
C1 . P1 . C2 . 105.10(9) yes
P1 . C1 . H11 . 111.1(18) no
P1 . C1 . H12 . 109.3(17) no
H11 . C1 . H12 . 106.5(25) no
P1 . C1 . H13 . 108.9(18) no
H11 . C1 . H13 . 109.5(24) no
H12 . C1 . H13 . 111.5(26) no
P1 . C2 . H21 . 113.0(24) no
P1 . C2 . H22 . 110.0(17) no
H21 . C2 . H22 . 106.0(21) no
P1 . C2 . H22 4_555 110.0(17) no
H21 . C2 . H22 4_555 106.0(21) no
H22 . C2 . H22 4_555 111.7(35) no

#CHECKCIF Alerts:
#061_ALERT B Tmax/Tmin Range Test RR' too large ...........       0.55
#The multiscan absorption procedure corrects for all effects leading to
#variation in the intensities of equivalent data. These might include decay
#and absorption by the crystal mmount.
#042_ALERT C Calc. and Rep. MoietyFormula Strings Differ ..          ?
#The one given is more chemically meaningful.
#062_ALERT C Rescale T(min) & T(max) by ...................       0.55
#Done
#125_ALERT C No _symmetry_space_group_name_Hall given .....          ?
#Corrected
#145_ALERT C su on beta     Small or Missing  (x 10000) ...         40 Deg.
#This is the value output by the data reduction/cell refinement program
#(Saint), although there is common agreement that such values are
#unrealistically small.
#164_ALERT C Nr. of Refined C-H H-Atoms in Heavy-At Struct.          7
#Information on these atoms was part of the reason for carrying out
#this determination. Hydrogens attached to the same atoms were given
#a common Uiso; similarity resratints were applied to the Ga-H and
#C-H primary bond distances.
#764_ALERT C Overcomplete CIF Bond list Detected (Rep/Expd)       1.33 Ratio
#Corrected.