#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:07:30 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179277 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/97/4319750.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_4319750
loop_
_publ_author_name
'Chia-Her Lin'
'Sue-Lein Wang'
_publ_section_title
;
 [(1S,2S)-H2DACH][Ga2(1S,2S-DACH)(HPO4)(PO4)2]: A Layered Chiral
 Gallophosphate Containing Chiral Ligand and Chiral Template
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2918
_journal_page_last               2921
_journal_paper_doi               10.1021/ic001234m
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         (C6H16N2)[Ga2(N2C6H14)(HPO4)(PO4)2]
_chemical_formula_sum            'C12 H31 Ga2 N4 O12 P3'
_chemical_formula_weight         655.76
_chemical_name_systematic
; 
diprotonated 1,2-diaminocyclohexane gallium phosphate 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.024(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.7802(8)
_cell_length_b                   9.1039(8)
_cell_length_c                   13.9235(12)
_cell_measurement_reflns_used    7562
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.19
_cell_volume                     1178.88(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0694
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7562
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    2.554
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
 The absorption correction was based on symmetry-equivalent reflections
 using the SADABS program. Sheldric, G. M. (1996). SADABS. Siemen Area Detector 
 Absorption Correction Software. University of Gottingen, Germany. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Lamellar
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.206
_refine_diff_density_min         -0.874
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(17)
_refine_ls_extinction_coef       0.0000(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         5299
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.571
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0846P)²+2.7368P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1400
_refine_ls_wR_factor_ref         0.1485
_reflns_number_gt                4392
_reflns_number_total             5299
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001234m.cif
_cod_data_source_block           '[(1S,2S)-H2DACH][Ga2(1S,2S-DACH)(HPO4)(PO4)2]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measure' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4319750
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, 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 0.39260(7) 0.97851(8) 0.07371(6) 0.01923(19) Uani 1 1 d . . .
Ga2 Ga 0.83457(7) 1.02894(8) 0.03174(6) 0.0212(2) Uani 1 1 d . . .
P1 P 0.73228(18) 0.9694(2) 0.21315(14) 0.0222(4) Uani 1 1 d . . .
P2 P 0.52502(18) 1.1293(2) -0.08369(15) 0.0190(4) Uani 1 1 d . . .
P3 P 0.07991(19) 0.8314(2) 0.01390(16) 0.0214(4) Uani 1 1 d . . .
O1 O 0.5930(5) 1.0256(7) 0.1415(4) 0.0282(12) Uani 1 1 d . . .
O2 O 0.8419(6) 0.9541(8) 0.1534(5) 0.0356(15) Uani 1 1 d . . .
O3 O 0.7905(7) 1.0892(7) 0.2969(5) 0.0370(14) Uani 1 1 d . . .
O4 O 0.7220(6) 0.8248(7) 0.2633(4) 0.0329(13) Uani 1 1 d . . .
O5 O 0.4040(5) 1.0611(6) -0.0526(4) 0.0220(12) Uani 1 1 d . . .
O6 O 0.4709(5) 1.1382(6) -0.2010(4) 0.0274(12) Uani 1 1 d . . .
O7 O 0.6557(5) 1.0266(7) -0.0596(4) 0.0262(11) Uani 1 1 d . . .
O8 O 0.5656(6) 1.2805(6) -0.0381(5) 0.0284(12) Uani 1 1 d . . .
O9 O 0.1851(5) 0.9508(6) 0.0052(4) 0.0243(12) Uani 1 1 d . . .
O10 O -0.0749(6) 0.8970(6) -0.0263(5) 0.0295(13) Uani 1 1 d . . .
O11 O 0.1108(6) 0.7675(7) 0.1167(5) 0.0345(14) Uani 1 1 d . . .
O12 O 0.0789(5) 0.7080(6) -0.0640(5) 0.0264(12) Uani 1 1 d . . .
N1 N 0.3477(7) 1.1875(8) 0.1206(6) 0.0309(15) Uani 1 1 d . . .
N2 N 0.3691(8) 0.9179(8) 0.2126(6) 0.0323(16) Uani 1 1 d . . .
N3 N -0.0923(7) 0.6356(8) 0.1825(5) 0.0313(15) Uani 1 1 d . . .
N4 N -0.2007(9) 0.3489(9) 0.2236(6) 0.0402(19) Uani 1 1 d . . .
C1 C 0.376(2) 1.1798(15) 0.2311(11) 0.095(6) Uani 1 1 d . . .
C2 C 0.3188(18) 1.0419(16) 0.2587(10) 0.079(5) Uani 1 1 d . . .
C3 C 0.365(2) 1.023(2) 0.3768(10) 0.102(6) Uani 1 1 d . . .
C4 C 0.356(3) 1.153(3) 0.4320(14) 0.154(11) Uani 1 1 d . . .
C5 C 0.410(3) 1.292(3) 0.3988(13) 0.133(9) Uani 1 1 d . . .
C6 C 0.366(2) 1.316(2) 0.2862(12) 0.101(6) Uani 1 1 d . . .
C7 C 0.0006(11) 0.5307(14) 0.2573(7) 0.053(3) Uani 1 1 d . . .
C8 C -0.0914(13) 0.4312(14) 0.2994(8) 0.062(4) Uani 1 1 d . . .
C9 C -0.118(3) 0.471(3) 0.3839(12) 0.174(14) Uani 1 1 d . . .
C10 C 0.003(2) 0.542(3) 0.4683(11) 0.131(9) Uani 1 1 d . . .
C11 C 0.079(2) 0.657(3) 0.4225(17) 0.150(12) Uani 1 1 d . . .
C12 C 0.109(2) 0.611(3) 0.3390(12) 0.131(10) Uani 1 1 d . . .
H1 H 0.7462 1.1851 0.2508 0.050 Uiso 1 1 d . . .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
O8 Ga1 O1 93.9(2) 2_645 . yes
O8 Ga1 O5 93.0(2) 2_645 . yes
O1 Ga1 O5 91.3(2) . . yes
O8 Ga1 O9 91.4(2) 2_645 . yes
O1 Ga1 O9 174.5(2) . . yes
O5 Ga1 O9 87.2(2) . . yes
O8 Ga1 N2 94.8(3) 2_645 . yes
O1 Ga1 N2 89.5(3) . . yes
O5 Ga1 N2 172.1(3) . . yes
O9 Ga1 N2 91.3(3) . . yes
O8 Ga1 N1 176.6(3) 2_645 . yes
O1 Ga1 N1 85.7(3) . . yes
O5 Ga1 N1 90.4(3) . . yes
O9 Ga1 N1 89.1(2) . . yes
N2 Ga1 N1 81.9(3) . . yes
O2 Ga2 O7 113.7(2) . . yes
O2 Ga2 O10 106.5(3) . 1_655 yes
O7 Ga2 O10 100.2(2) . 1_655 yes
O2 Ga2 O12 103.0(3) . 2_655 yes
O7 Ga2 O12 117.0(3) . 2_655 yes
O10 Ga2 O12 116.4(3) 1_655 2_655 yes
O1 P1 O4 115.3(3) . . yes
O1 P1 O2 107.9(3) . . yes
O4 P1 O2 109.0(4) . . yes
O1 P1 O3 107.6(4) . . yes
O4 P1 O3 108.9(4) . . yes
O2 P1 O3 107.9(4) . . yes
O5 P2 O8 112.3(3) . . yes
O5 P2 O7 111.1(3) . . yes
O8 P2 O7 111.7(3) . . yes
O5 P2 O6 106.2(3) . . yes
O8 P2 O6 110.6(3) . . yes
O7 P2 O6 104.6(3) . . yes
O11 P3 O9 114.4(3) . . yes
O11 P3 O12 110.1(4) . . yes
O9 P3 O12 108.5(3) . . yes
O11 P3 O10 112.4(3) . . yes
O9 P3 O10 107.6(3) . . yes
O12 P3 O10 103.3(3) . . yes
P1 O1 Ga1 144.7(4) . . yes
P1 O2 Ga2 129.4(4) . . yes
P2 O5 Ga1 133.2(3) . . yes
P2 O7 Ga2 134.6(4) . . yes
P2 O8 Ga1 141.5(4) . 2_655 yes
P3 O9 Ga1 132.0(3) . . yes
P3 O10 Ga2 130.1(4) . 1_455 yes
P3 O12 Ga2 124.7(4) . 2_645 yes
C1 N1 Ga1 106.9(7) . . yes
C2 N2 Ga1 110.6(7) . . yes
N1 C1 C2 110.4(11) . . yes
N1 C1 C6 118.7(14) . . yes
C2 C1 C6 119.1(13) . . yes
N2 C2 C1 109.7(10) . . yes
N2 C2 C3 110.5(13) . . yes
C1 C2 C3 110.8(12) . . yes
C4 C3 C2 115.4(16) . . yes
C3 C4 C5 116.6(16) . . yes
C4 C5 C6 115.1(17) . . yes
C1 C6 C5 112.3(16) . . yes
C12 C7 N3 110.8(13) . . yes
C12 C7 C8 111.5(10) . . yes
N3 C7 C8 110.2(9) . . yes
C9 C8 N4 118.6(12) . . yes
C9 C8 C7 118.8(12) . . yes
N4 C8 C7 114.7(9) . . yes
C8 C9 C10 118.2(16) . . yes
C11 C10 C9 109.3(14) . . yes
C12 C11 C10 114.2(18) . . yes
C11 C12 C7 121.1(16) . . yes
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 O8 1.946(5) 2_645 yes
Ga1 O1 1.942(5) . yes
Ga1 O5 1.948(5) . yes
Ga1 O9 1.973(5) . yes
Ga1 N2 2.091(7) . yes
Ga1 N1 2.101(7) . yes
Ga2 O2 1.806(6) . yes
Ga2 O7 1.817(5) . yes
Ga2 O10 1.823(6) 1_655 yes
Ga2 O12 1.828(5) 2_655 yes
P1 O1 1.507(5) . yes
P1 O4 1.508(6) . yes
P1 O2 1.553(6) . yes
P1 O3 1.570(6) . yes
P2 O5 1.513(5) . yes
P2 O8 1.516(6) . yes
P2 O7 1.535(5) . yes
P2 O6 1.555(6) . yes
P3 O11 1.486(7) . yes
P3 O9 1.528(5) . yes
P3 O12 1.559(6) . yes
P3 O10 1.561(5) . yes
O8 Ga1 1.946(5) 2_655 no
O10 Ga2 1.823(6) 1_455 no
O12 Ga2 1.828(5) 2_645 no
N1 C1 1.478(15) . yes
N2 C2 1.457(15) . yes
N3 C7 1.495(12) . yes
N4 C8 1.456(12) . yes
C1 C2 1.474(19) . yes
C1 C6 1.475(19) . yes
C2 C3 1.573(18) . yes
C3 C4 1.43(3) . yes
C4 C5 1.50(3) . yes
C5 C6 1.51(2) . yes
C7 C12 1.486(18) . yes
C7 C8 1.517(14) . yes
C8 C9 1.33(2) . yes
C9 C10 1.53(2) . yes
C10 C11 1.53(3) . yes
C11 C12 1.35(3) . yes
