# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_email       jyao@mail.ipc.ac.cn
_publ_contact_author_name        'Jiyong Yao'
_publ_author_name                'Jiyong Yao'

data_final
_database_code_depnum_ccdc_archive 'CCDC 835526'
#TrackingRef '- NaGe3P3.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ge3 Na P3'
_chemical_formula_weight         333.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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           orthorhombic
_symmetry_space_group_name_H-M   Pmc21

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

_cell_length_a                   3.6276(7)
_cell_length_b                   8.4068(17)
_cell_length_c                   10.332(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     315.09(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    985
_cell_measurement_theta_min      2.4227
_cell_measurement_theta_max      29.1190

_exptl_crystal_description       Platele
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.005
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    3.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             304
_exptl_absorpt_coefficient_mu    14.907
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.17
_exptl_absorpt_correction_T_max  0.52
_exptl_absorpt_process_details   'face indexed'

_exptl_special_details           ?

_diffrn_ambient_temperature      93
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_measurement_device_type  'Rigaku AFC10 diffractometer'
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3132
_diffrn_reflns_av_R_equivalents  0.0777
_diffrn_reflns_av_sigmaI/netI    0.0992
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.12
_diffrn_reflns_theta_max         29.10
_reflns_number_total             931
_reflns_number_gt                722
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  Diamond

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00065(5)
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(3)
_refine_ls_number_reflns         931
_refine_ls_number_parameters     43
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.0842
_refine_ls_wR_factor_gt          0.0739
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.057
_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
Na1 Na 0.0000 0.3700(7) 0.0012(7) 0.0479(19) Uani 1 2 d S . .
Ge1 Ge 0.5000 0.18517(15) 0.41319(11) 0.0122(3) Uani 1 2 d S . .
Ge2 Ge 0.0000 0.70575(18) 0.22415(13) 0.0178(4) Uani 1 2 d S . .
Ge3 Ge 0.0000 0.00306(18) 0.14629(14) 0.0128(3) Uani 1 2 d S . .
P1 P 0.0000 0.2346(4) 0.2770(3) 0.0124(7) Uani 1 2 d S . .
P2 P 0.5000 0.0677(4) 0.0064(3) 0.0140(7) Uani 1 2 d S . .
P3 P 0.5000 0.6288(4) 0.0782(3) 0.0177(8) Uani 1 2 d S . .

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
Na1 0.053(5) 0.033(4) 0.058(5) -0.006(4) 0.000 0.000
Ge1 0.0084(7) 0.0170(7) 0.0110(7) 0.0012(6) 0.000 0.000
Ge2 0.0093(8) 0.0235(8) 0.0205(8) -0.0048(7) 0.000 0.000
Ge3 0.0078(6) 0.0173(7) 0.0133(6) -0.0019(6) 0.000 0.000
P1 0.0106(18) 0.0158(18) 0.0107(15) -0.0028(13) 0.000 0.000
P2 0.0091(17) 0.021(2) 0.0117(16) -0.0061(14) 0.000 0.000
P3 0.023(2) 0.0172(19) 0.0128(17) 0.0030(14) 0.000 0.000

_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
Na1 Ge2 2.933(8) 2_564 ?
Na1 P3 2.942(6) . ?
Na1 P3 2.942(6) 1_455 ?
Na1 P1 3.068(8) . ?
Na1 P2 3.122(6) 1_455 ?
Na1 P2 3.122(6) . ?
Na1 Ge3 3.430(7) . ?
Na1 Na1 3.6276(7) 1_655 ?
Na1 Na1 3.6276(7) 1_455 ?
Ge1 P3 2.314(4) 2_665 ?
Ge1 P1 2.333(2) . ?
Ge1 P1 2.333(2) 1_655 ?
Ge1 P2 2.334(4) 2_655 ?
Ge2 P3 2.446(2) 1_455 ?
Ge2 P3 2.446(2) . ?
Ge2 Ge3 2.626(2) 1_565 ?
Ge2 Na1 2.933(8) 2_565 ?
Ge3 P1 2.369(3) . ?
Ge3 P2 2.382(2) 1_455 ?
Ge3 P2 2.382(2) . ?
Ge3 Ge2 2.626(2) 1_545 ?
P1 Ge1 2.333(2) 1_455 ?
P2 Ge1 2.334(4) 2_654 ?
P2 Ge3 2.382(2) 1_655 ?
P2 Na1 3.122(6) 1_655 ?
P3 Ge1 2.314(4) 2_664 ?
P3 Ge2 2.446(2) 1_655 ?
P3 Na1 2.942(6) 1_655 ?

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
Ge2 Na1 P3 115.1(2) 2_564 . ?
Ge2 Na1 P3 115.1(2) 2_564 1_455 ?
P3 Na1 P3 76.12(17) . 1_455 ?
Ge2 Na1 P1 145.7(2) 2_564 . ?
P3 Na1 P1 91.3(2) . . ?
P3 Na1 P1 91.3(2) 1_455 . ?
Ge2 Na1 P2 80.80(16) 2_564 1_455 ?
P3 Na1 P2 162.8(3) . 1_455 ?
P3 Na1 P2 103.83(8) 1_455 1_455 ?
P1 Na1 P2 71.47(16) . 1_455 ?
Ge2 Na1 P2 80.80(16) 2_564 . ?
P3 Na1 P2 103.83(8) . . ?
P3 Na1 P2 162.8(3) 1_455 . ?
P1 Na1 P2 71.47(16) . . ?
P2 Na1 P2 71.03(15) 1_455 . ?
Ge2 Na1 Ge3 103.37(18) 2_564 . ?
P3 Na1 Ge3 123.15(19) . . ?
P3 Na1 Ge3 123.15(19) 1_455 . ?
P1 Na1 Ge3 42.31(11) . . ?
P2 Na1 Ge3 42.31(9) 1_455 . ?
P2 Na1 Ge3 42.31(9) . . ?
Ge2 Na1 Na1 90.0 2_564 1_655 ?
P3 Na1 Na1 51.94(9) . 1_655 ?
P3 Na1 Na1 128.06(9) 1_455 1_655 ?
P1 Na1 Na1 90.0 . 1_655 ?
P2 Na1 Na1 125.51(7) 1_455 1_655 ?
P2 Na1 Na1 54.49(7) . 1_655 ?
Ge3 Na1 Na1 90.0 . 1_655 ?
Ge2 Na1 Na1 90.0 2_564 1_455 ?
P3 Na1 Na1 128.06(8) . 1_455 ?
P3 Na1 Na1 51.94(9) 1_455 1_455 ?
P1 Na1 Na1 90.0 . 1_455 ?
P2 Na1 Na1 54.49(7) 1_455 1_455 ?
P2 Na1 Na1 125.51(7) . 1_455 ?
Ge3 Na1 Na1 90.0 . 1_455 ?
Na1 Na1 Na1 180.0 1_655 1_455 ?
P3 Ge1 P1 108.91(10) 2_665 . ?
P3 Ge1 P1 108.91(10) 2_665 1_655 ?
P1 Ge1 P1 102.06(14) . 1_655 ?
P3 Ge1 P2 108.15(13) 2_665 2_655 ?
P1 Ge1 P2 114.28(9) . 2_655 ?
P1 Ge1 P2 114.28(9) 1_655 2_655 ?
P3 Ge2 P3 95.75(13) 1_455 . ?
P3 Ge2 Ge3 93.60(9) 1_455 1_565 ?
P3 Ge2 Ge3 93.60(9) . 1_565 ?
P3 Ge2 Na1 122.98(10) 1_455 2_565 ?
P3 Ge2 Na1 122.98(10) . 2_565 ?
Ge3 Ge2 Na1 120.39(13) 1_565 2_565 ?
P1 Ge3 P2 99.11(11) . 1_455 ?
P1 Ge3 P2 99.11(11) . . ?
P2 Ge3 P2 99.18(13) 1_455 . ?
P1 Ge3 Ge2 127.41(11) . 1_545 ?
P2 Ge3 Ge2 113.78(9) 1_455 1_545 ?
P2 Ge3 Ge2 113.78(9) . 1_545 ?
P1 Ge3 Na1 60.67(16) . . ?
P2 Ge3 Na1 61.93(10) 1_455 . ?
P2 Ge3 Na1 61.93(10) . . ?
Ge2 Ge3 Na1 171.93(13) 1_545 . ?
Ge1 P1 Ge1 102.06(14) . 1_455 ?
Ge1 P1 Ge3 101.38(11) . . ?
Ge1 P1 Ge3 101.38(11) 1_455 . ?
Ge1 P1 Na1 128.77(7) . . ?
Ge1 P1 Na1 128.77(7) 1_455 . ?
Ge3 P1 Na1 77.02(16) . . ?
Ge1 P2 Ge3 92.43(11) 2_654 1_655 ?
Ge1 P2 Ge3 92.43(11) 2_654 . ?
Ge3 P2 Ge3 99.18(13) 1_655 . ?
Ge1 P2 Na1 137.24(12) 2_654 1_655 ?
Ge3 P2 Na1 75.75(12) 1_655 1_655 ?
Ge3 P2 Na1 129.68(17) . 1_655 ?
Ge1 P2 Na1 137.24(12) 2_654 . ?
Ge3 P2 Na1 129.68(17) 1_655 . ?
Ge3 P2 Na1 75.75(12) . . ?
Na1 P2 Na1 71.03(15) 1_655 . ?
Ge1 P3 Ge2 106.00(11) 2_664 1_655 ?
Ge1 P3 Ge2 106.00(11) 2_664 . ?
Ge2 P3 Ge2 95.75(13) 1_655 . ?
Ge1 P3 Na1 107.48(18) 2_664 . ?
Ge2 P3 Na1 145.04(18) 1_655 . ?
Ge2 P3 Na1 84.56(11) . . ?
Ge1 P3 Na1 107.48(18) 2_664 1_655 ?
Ge2 P3 Na1 84.56(11) 1_655 1_655 ?
Ge2 P3 Na1 145.04(18) . 1_655 ?
Na1 P3 Na1 76.12(17) . 1_655 ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        29.10
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.296
_refine_diff_density_min         -1.797
_refine_diff_density_rms         0.318