#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:06:48 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179231 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/51/4315129.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4315129
loop_
_publ_author_name
'Martin P. Attfield'
'Zhanhui Yuan'
'Howard G. Harvey'
'William Clegg'
_publ_section_title
;
 Structural Variety within Gallium Diphosphonates Affected by the Organic
 Linker Length
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2656
_journal_page_last               2666
_journal_paper_doi               10.1021/ic901651d
_journal_volume                  49
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C6 H13 Ga3 O13 P4'
_chemical_formula_sum            'C6 H13 Ga3 O13 P4'
_chemical_formula_weight         626.2
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2009-07-07T15:25:27-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.990(8)
_cell_length_b                   10.022(2)
_cell_length_c                   8.3093(17)
_cell_measurement_reflns_used    62
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.5
_cell_volume                     3163.6(11)
_computing_cell_refinement       DIRAX
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL, WinGX and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.057
_diffrn_reflns_av_unetI/netI     0.0871
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5939
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         4.21
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.548
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.629
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.2
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.46(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         2504
_refine_ls_number_restraints     165
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0314P)²+38.4028P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0962
_reflns_number_gt                2059
_reflns_number_total             2504
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic901651d_si_002_1.cif
_cod_data_source_block           zy6_Ga3OH(O3PC3H6PO3)2
_cod_database_code               4315129
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
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
Ga1 Ga 0.37808(3) -0.16736(10) 0.70301(12) 0.0047(3) Uani 1 1 d U . .
Ga2 Ga 0.40678(3) -0.31343(11) 1.17572(12) 0.0054(3) Uani 1 1 d U . .
Ga3 Ga 0.30992(3) 0.04288(12) 0.74119(14) 0.0113(3) Uani 1 1 d U . .
P1 P 0.42532(7) -0.4051(3) 1.5385(3) 0.0045(5) Uani 1 1 d U . .
P2 P 0.42528(7) -0.0533(3) 0.9944(3) 0.0048(4) Uani 1 1 d U . .
P3 P 0.33359(8) -0.2719(3) 1.0265(3) 0.0068(4) Uani 1 1 d U . .
P4 P 0.29925(7) -0.1917(3) 0.5492(3) 0.0073(5) Uani 1 1 d U . .
O1 O 0.3517(2) -0.2764(7) 0.8657(9) 0.0070(6) Uani 1 1 d U . .
O2 O 0.33873(18) -0.1846(7) 0.5519(8) 0.0070(6) Uani 1 1 d U . .
O3 O 0.39642(19) -0.3359(7) 0.6316(8) 0.0073(12) Uani 1 1 d U . .
O4 O 0.4177(2) -0.1291(7) 0.8391(8) 0.0056(5) Uani 1 1 d U . .
O5 O 0.39885(17) 0.0572(6) 1.0263(8) 0.0048(6) Uani 1 1 d U . .
O6 O 0.42733(18) -0.1527(7) 1.1372(7) 0.0050(6) Uani 1 1 d U . .
O7 O 0.42834(19) -0.3563(7) 1.3641(8) 0.0050(6) Uani 1 1 d U . .
O8 O 0.41988(18) -0.5584(6) 1.5315(8) 0.0047(7) Uani 1 1 d U . .
O9 O 0.35905(17) -0.2960(6) 1.1707(9) 0.0071(6) Uani 1 1 d U . .
O10 O 0.31328(18) -0.1387(7) 1.0546(8) 0.0070(6) Uani 1 1 d U . .
O11 O 0.28562(19) -0.1424(7) 0.3835(8) 0.0075(6) Uani 1 1 d U . .
O12 O 0.28312(16) -0.1049(6) 0.6851(8) 0.0078(6) Uani 1 1 d U . .
O13 O 0.35474(18) -0.0071(7) 0.7874(8) 0.0067(10) Uani 1 1 d U . .
C1 C 0.4672(3) -0.3737(11) 1.6365(12) 0.0064(12) Uani 1 1 d U . .
H6A H 0.4688 -0.2773 1.6616 0.008 Uiso 1 1 calc R . .
H6B H 0.4676 -0.4226 1.74 0.008 Uiso 1 1 calc R . .
C2 C 0.5 -0.4134(15) 1.5401(18) 0.0063(13) Uani 1 2 d SU . .
H7A H 0.5 -0.5109 1.5206 0.008 Uiso 1 2 calc SR . .
H7B H 0.5 -0.3674 1.4346 0.008 Uiso 1 2 calc SR . .
C3 C 0.4672(3) 0.0238(10) 0.9863(13) 0.0062(11) Uani 1 1 d U . .
H5A H 0.4671 0.0866 0.8943 0.007 Uiso 1 1 calc R . .
H5B H 0.47 0.0778 1.0852 0.007 Uiso 1 1 calc R . .
C4 C 0.5 -0.0655(15) 0.9698(18) 0.0061(13) Uani 1 2 d SU . .
H2A H 0.5 -0.1347 1.0548 0.007 Uiso 1 2 calc SR . .
H2B H 0.5 -0.1104 0.8637 0.007 Uiso 1 2 calc SR . .
C5 C 0.3003(3) -0.3971(10) 1.0424(13) 0.0091(13) Uani 1 1 d U . .
H1A H 0.2888 -0.3885 1.1487 0.011 Uiso 1 1 calc R . .
H1B H 0.2823 -0.3803 0.959 0.011 Uiso 1 1 calc R . .
C6 C 0.3136(3) -0.5397(10) 1.0239(13) 0.0092(13) Uani 1 1 d U . .
H3A H 0.3344 -0.5536 1.0936 0.011 Uiso 1 1 calc R . .
H3B H 0.3208 -0.5557 0.911 0.011 Uiso 1 1 calc R . .
C7 C 0.2837(3) -0.3600(10) 0.5723(13) 0.0096(16) Uani 1 1 d U . .
H4A H 0.2767 -0.3756 0.6855 0.012 Uiso 1 1 calc R . .
H4B H 0.2628 -0.3744 0.5031 0.012 Uiso 1 1 calc R . .
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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O3 Ga1 O4 94.2(3) . . ?
O3 Ga1 O2 90.1(3) . . ?
O4 Ga1 O2 172.8(3) . . ?
O3 Ga1 O13 173.2(3) . . ?
O4 Ga1 O13 88.9(3) . . ?
O2 Ga1 O13 87.5(3) . . ?
O3 Ga1 O5 96.6(3) . 3_554 ?
O4 Ga1 O5 90.7(3) . 3_554 ?
O2 Ga1 O5 83.0(3) . 3_554 ?
O13 Ga1 O5 89.4(3) . 3_554 ?
O3 Ga1 O1 84.9(3) . . ?
O4 Ga1 O1 96.0(3) . . ?
O2 Ga1 O1 90.2(3) . . ?
O13 Ga1 O1 88.8(3) . . ?
O5 Ga1 O1 173.0(3) 3_554 . ?
O7 Ga2 O6 99.6(3) . . ?
O7 Ga2 O9 119.4(3) . . ?
O6 Ga2 O9 109.8(3) . . ?
O7 Ga2 O8 106.0(3) . 3_544 ?
O6 Ga2 O8 113.0(3) . 3_544 ?
O9 Ga2 O8 108.9(3) . 3_544 ?
O11 Ga3 O13 119.6(3) 3 . ?
O11 Ga3 O10 107.6(3) 3 3_554 ?
O13 Ga3 O10 105.0(3) . 3_554 ?
O11 Ga3 O12 109.0(3) 3 . ?
O13 Ga3 O12 110.3(3) . . ?
O10 Ga3 O12 104.1(3) 3_554 . ?
O3 P1 O7 113.1(4) 1_556 . ?
O3 P1 O8 112.1(4) 1_556 . ?
O7 P1 O8 106.9(4) . . ?
O3 P1 C1 109.1(4) 1_556 . ?
O7 P1 C1 107.6(4) . . ?
O8 P1 C1 107.8(5) . . ?
O5 P2 O4 112.8(4) . . ?
O5 P2 O6 111.6(4) . . ?
O4 P2 O6 109.7(4) . . ?
O5 P2 C3 106.4(4) . . ?
O4 P2 C3 110.7(5) . . ?
O6 P2 C3 105.3(5) . . ?
O1 P3 O9 113.2(4) . . ?
O1 P3 O10 112.6(4) . . ?
O9 P3 O10 108.9(4) . . ?
O1 P3 C5 111.7(5) . . ?
O9 P3 C5 105.9(4) . . ?
O10 P3 C5 103.9(4) . . ?
O2 P4 O12 110.9(4) . . ?
O2 P4 O11 109.4(4) . . ?
O12 P4 O11 109.6(4) . . ?
O2 P4 C7 111.8(5) . . ?
O12 P4 C7 108.6(4) . . ?
O11 P4 C7 106.5(5) . . ?
P3 O1 Ga1 144.2(4) . . ?
P4 O2 Ga1 140.9(5) . . ?
P1 O3 Ga1 145.6(5) 1_554 . ?
P2 O4 Ga1 138.1(5) . . ?
P2 O5 Ga1 142.3(4) . 3 ?
P2 O6 Ga2 133.0(4) . . ?
P1 O7 Ga2 148.8(5) . . ?
P1 O8 Ga2 135.1(4) . 3_545 ?
P3 O9 Ga2 130.5(5) . . ?
P3 O10 Ga3 127.7(4) . 3 ?
P4 O11 Ga3 126.0(4) . 3_554 ?
P4 O12 Ga3 114.4(4) . . ?
Ga3 O13 Ga1 125.0(4) . . ?
C2 C1 P1 115.6(7) . . ?
C1 C2 C1 108.6(12) 4_655 . ?
C4 C3 P2 118.5(8) . . ?
C3 C4 C3 108.1(12) 4_655 . ?
C6 C5 P3 114.6(7) . . ?
C5 C6 C7 109.5(8) . 3_545 ?
C6 C7 P4 109.6(7) 3_544 . ?
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
Ga1 O3 1.921(7) . ?
Ga1 O4 1.923(7) . ?
Ga1 O2 1.960(7) . ?
Ga1 O13 1.964(7) . ?
Ga1 O5 1.999(7) 3_554 ?
Ga1 O1 2.006(7) . ?
Ga2 O7 1.818(7) . ?
Ga2 O6 1.818(7) . ?
Ga2 O9 1.822(7) . ?
Ga2 O8 1.826(6) 3_544 ?
Ga3 O11 1.801(7) 3 ?
Ga3 O13 1.816(7) . ?
Ga3 O10 1.828(7) 3_554 ?
Ga3 O12 1.856(7) . ?
P1 O3 1.512(7) 1_556 ?
P1 O7 1.533(7) . ?
P1 O8 1.552(7) . ?
P1 C1 1.816(10) . ?
P2 O5 1.518(7) . ?
P2 O4 1.525(7) . ?
P2 O6 1.551(7) . ?
P2 C3 1.770(10) . ?
P3 O1 1.503(7) . ?
P3 O9 1.559(8) . ?
P3 O10 1.560(7) . ?
P3 C5 1.785(10) . ?
P4 O2 1.502(7) . ?
P4 O12 1.552(7) . ?
P4 O11 1.552(7) . ?
P4 C7 1.798(11) . ?
O3 P1 1.512(7) 1_554 ?
O5 Ga1 1.999(7) 3 ?
O8 Ga2 1.826(6) 3_545 ?
O10 Ga3 1.828(7) 3 ?
O11 Ga3 1.801(7) 3_554 ?
C1 C2 1.533(13) . ?
C2 C1 1.533(13) 4_655 ?
C3 C4 1.541(13) . ?
C4 C3 1.541(13) 4_655 ?
C5 C6 1.524(14) . ?
C6 C7 1.570(14) 3_545 ?
C7 C6 1.570(14) 3_544 ?
