#------------------------------------------------------------------------------
#$Date: 2016-05-06 04:50:20 +0300 (Fri, 06 May 2016) $
#$Revision: 182737 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/87/7038764.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_7038764
loop_
_publ_author_name
'Hou, Xiaomin'
'Tang, Si-Fu'
_publ_section_title
;
 Speciation of metal phosphonates with the assistance of weak
 interactions.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7349
_journal_page_last               7359
_journal_paper_doi               10.1039/c6dt00643d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C17 H30 Cd N2 O13 P2'
_chemical_formula_weight         644.77
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-03-09 deposited with the CCDC.
2016-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.3240(17)
_cell_length_b                   21.707(2)
_cell_length_c                   16.2613(18)
_cell_measurement_reflns_used    24429
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1.88
_cell_volume                     5056.1(9)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1044
_diffrn_reflns_av_unetI/netI     0.0925
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19301
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.876
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.056
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_description       block
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.372
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4424
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.888
_refine_ls_R_factor_all          0.1308
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0584P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1175
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2286
_reflns_number_total             4424
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt00643d2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7038759--7038764.cif.'
_cod_original_cell_volume        5056.1(10)
_cod_database_code               7038764
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Cd1 Cd 0.58552(3) 0.04760(2) 0.05345(3) 0.02531(15) Uani 1 1 d . .
O1W O 0.5803(3) 0.12877(18) -0.0364(2) 0.0357(11) Uani 1 1 d . .
H1W H 0.6172 0.1559 -0.0555 0.043 Uiso 1 1 d R U
H2W H 0.5300 0.1165 -0.0588 0.043 Uiso 1 1 d R U
O1 O 0.7532(2) 0.05925(15) 0.4549(2) 0.0174(9) Uani 1 1 d . U
H1A H 0.7596 0.0379 0.4961 0.026 Uiso 1 1 calc R U
O2 O 0.8660(3) 0.14058(18) 0.4083(3) 0.0337(11) Uani 1 1 d . .
O2W O 0.7292(3) 0.2059(2) -0.0464(3) 0.0520(14) Uani 1 1 d . .
H3W H 0.7599 0.2162 -0.0890 0.062 Uiso 1 1 d R U
H4W H 0.6942 0.2150 -0.0061 0.062 Uiso 1 1 d R U
O3 O 0.9250(3) 0.03831(16) 0.4657(2) 0.0213(10) Uani 1 1 d . .
O3W O 0.9387(3) 0.2136(2) 0.5243(3) 0.0512(14) Uani 1 1 d . .
H5W H 0.8992 0.2362 0.5491 0.061 Uiso 1 1 d R U
H6W H 0.9926 0.2090 0.5454 0.061 Uiso 1 1 d R U
O4 O 0.8048(3) 0.14562(19) 0.0837(3) 0.0388(12) Uani 1 1 d . .
O4W O 0.9984(4) 0.1663(2) -0.0268(3) 0.0638(16) Uani 1 1 d . .
H7W H 0.9709 0.1800 -0.0694 0.077 Uiso 1 1 d R U
H8W H 1.0577 0.1665 -0.0263 0.077 Uiso 1 1 d R U
O5 O 0.9117(3) 0.0663(2) 0.0228(3) 0.0394(11) Uani 1 1 d . .
H5A H 0.9372 0.0993 0.0124 0.059 Uiso 1 1 calc R U
O5W O 0.6899(4) 0.1814(2) 0.5297(3) 0.0606(16) Uani 1 1 d . .
H9W H 0.7375 0.1585 0.5226 0.073 Uiso 1 1 d R U
H10W H 0.6806 0.1906 0.4795 0.073 Uiso 1 1 d R U
O6 O 0.7427(3) 0.04560(18) 0.0249(2) 0.0295(10) Uani 1 1 d . .
O6W O 0.8103(4) 0.2545(2) 0.1526(3) 0.0572(15) Uani 1 1 d . .
H11W H 0.8689 0.2522 0.1602 0.069 Uiso 1 1 d R U
H12W H 0.7792 0.2809 0.1253 0.069 Uiso 1 1 d R U
O7W O 0.8301(4) 0.2493(2) 0.3277(3) 0.0677(17) Uani 1 1 d . .
H13W H 0.8010 0.2393 0.2841 0.081 Uiso 1 1 d R U
H14W H 0.8887 0.2503 0.3359 0.081 Uiso 1 1 d R U
N1 N 0.5929(4) -0.0135(2) 0.1695(3) 0.0291(12) Uani 1 1 d . .
N2 N 0.5825(4) 0.1099(2) 0.1703(3) 0.0320(13) Uani 1 1 d . .
P1 P 0.85204(12) 0.07302(8) 0.41591(10) 0.0230(4) Uani 1 1 d . .
P2 P 0.81941(12) 0.07854(8) 0.07179(10) 0.0252(4) Uani 1 1 d . .
C1 C 0.8528(5) -0.1280(3) 0.2371(4) 0.050(2) Uani 1 1 d . .
H1B H 0.8637 -0.1421 0.1819 0.075 Uiso 1 1 calc R U
H1C H 0.7949 -0.1446 0.2568 0.075 Uiso 1 1 calc R U
H1D H 0.9029 -0.1414 0.2720 0.075 Uiso 1 1 calc R U
C2 C 0.8480(5) -0.0590(3) 0.2377(4) 0.0312(17) Uani 1 1 d . .
C3 C 0.8518(4) -0.0276(3) 0.3119(4) 0.0263(16) Uani 1 1 d . .
H3A H 0.8580 -0.0499 0.3604 0.032 Uiso 1 1 calc R U
C4 C 0.8467(4) 0.0371(3) 0.3158(4) 0.0232(15) Uani 1 1 d . .
C5 C 0.8375(4) 0.0700(3) 0.2422(4) 0.0226(14) Uani 1 1 d . .
H5B H 0.8338 0.1128 0.2435 0.027 Uiso 1 1 calc R U
C6 C 0.8339(4) 0.0396(3) 0.1677(4) 0.0238(15) Uani 1 1 d . .
C7 C 0.8401(4) -0.0249(3) 0.1673(4) 0.0319(17) Uani 1 1 d . .
H7A H 0.8388 -0.0453 0.1170 0.038 Uiso 1 1 calc R U
C8 C 0.5982(5) -0.0754(3) 0.1654(4) 0.0352(17) Uani 1 1 d . .
H8A H 0.6003 -0.0943 0.1141 0.042 Uiso 1 1 calc R U
C9 C 0.6005(5) -0.1112(3) 0.2341(5) 0.047(2) Uani 1 1 d . .
H9A H 0.6026 -0.1538 0.2294 0.057 Uiso 1 1 calc R U
C10 C 0.5997(5) -0.0842(3) 0.3096(5) 0.052(2) Uani 1 1 d . .
H10A H 0.6020 -0.1081 0.3571 0.063 Uiso 1 1 calc R U
C11 C 0.5956(5) -0.0209(3) 0.3144(4) 0.0419(18) Uani 1 1 d . .
H11A H 0.5955 -0.0016 0.3654 0.050 Uiso 1 1 calc R U
C12 C 0.5916(5) 0.0139(3) 0.2430(4) 0.0293(15) Uani 1 1 d . .
C13 C 0.5863(5) 0.0822(3) 0.2440(4) 0.0308(15) Uani 1 1 d . .
C14 C 0.5832(6) 0.1156(3) 0.3161(5) 0.051(2) Uani 1 1 d . .
H14A H 0.5857 0.0959 0.3668 0.061 Uiso 1 1 calc R U
C15 C 0.5765(6) 0.1789(4) 0.3112(5) 0.065(3) Uani 1 1 d . .
H15A H 0.5753 0.2024 0.3591 0.078 Uiso 1 1 calc R U
C16 C 0.5714(6) 0.2071(4) 0.2365(5) 0.061(2) Uani 1 1 d . .
H16A H 0.5652 0.2496 0.2325 0.073 Uiso 1 1 calc R U
C17 C 0.5757(5) 0.1713(3) 0.1677(5) 0.050(2) Uani 1 1 d . .
H17A H 0.5739 0.1904 0.1166 0.060 Uiso 1 1 calc R U
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'
Cd Cd -0.8075 1.2024 '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
O1W Cd1 O6 85.26(15) . .
O1W Cd1 N1 164.75(16) . .
O6 Cd1 N1 96.29(17) . .
O1W Cd1 O3 87.11(14) . 6_556
O6 Cd1 O3 159.74(13) . 6_556
N1 Cd1 O3 95.99(16) . 6_556
O1W Cd1 N2 94.19(16) . .
O6 Cd1 N2 101.17(17) . .
N1 Cd1 N2 70.61(17) . .
O3 Cd1 N2 98.07(16) 6_556 .
O1W Cd1 O3 102.75(13) . 2_654
O6 Cd1 O3 85.71(14) . 2_654
N1 Cd1 O3 92.50(15) . 2_654
O3 Cd1 O3 77.72(14) 6_556 2_654
N2 Cd1 O3 162.24(15) . 2_654
P1 O3 Cd1 124.4(2) . 6_656
P1 O3 Cd1 132.2(2) . 2_655
Cd1 O3 Cd1 102.28(14) 6_656 2_655
P2 O6 Cd1 126.8(2) . .
C12 N1 C8 119.3(6) . .
C12 N1 Cd1 118.4(4) . .
C8 N1 Cd1 122.4(4) . .
C17 N2 C13 118.6(6) . .
C17 N2 Cd1 123.6(5) . .
C13 N2 Cd1 117.8(4) . .
O2 P1 O3 116.2(2) . .
O2 P1 O1 109.9(2) . .
O3 P1 O1 108.0(2) . .
O2 P1 C4 110.9(3) . .
O3 P1 C4 107.1(2) . .
O1 P1 C4 104.0(2) . .
O4 P2 O6 115.2(3) . .
O4 P2 O5 110.6(3) . .
O6 P2 O5 106.0(2) . .
O4 P2 C6 111.5(3) . .
O6 P2 C6 107.5(3) . .
O5 P2 C6 105.4(3) . .
C7 C2 C3 117.8(5) . .
C7 C2 C1 122.5(6) . .
C3 C2 C1 119.7(6) . .
C2 C3 C4 121.8(6) . .
C5 C4 C3 118.4(5) . .
C5 C4 P1 123.6(5) . .
C3 C4 P1 118.0(5) . .
C6 C5 C4 120.6(5) . .
C5 C6 C7 118.7(6) . .
C5 C6 P2 122.9(5) . .
C7 C6 P2 118.4(5) . .
C2 C7 C6 122.7(6) . .
N1 C8 C9 122.0(7) . .
C10 C9 C8 119.7(7) . .
C9 C10 C11 118.7(7) . .
C10 C11 C12 119.9(7) . .
N1 C12 C11 120.4(6) . .
N1 C12 C13 117.0(6) . .
C11 C12 C13 122.6(6) . .
N2 C13 C14 121.5(6) . .
N2 C13 C12 116.2(6) . .
C14 C13 C12 122.3(6) . .
C13 C14 C15 118.5(7) . .
C16 C15 C14 120.1(7) . .
C15 C16 C17 118.2(7) . .
N2 C17 C16 123.1(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 O1W 2.290(4) .
Cd1 O6 2.300(4) .
Cd1 N1 2.309(5) .
Cd1 O3 2.329(4) 6_556
Cd1 N2 2.333(5) .
Cd1 O3 2.353(3) 2_654
O1 P1 1.580(4) .
O2 P1 1.485(4) .
O3 P1 1.521(4) .
O3 Cd1 2.329(4) 6_656
O3 Cd1 2.353(3) 2_655
O4 P2 1.484(4) .
O5 P2 1.566(5) .
O6 P2 1.516(4) .
N1 C12 1.336(7) .
N1 C8 1.348(7) .
N2 C17 1.336(7) .
N2 C13 1.341(8) .
P1 C4 1.807(6) .
P2 C6 1.787(6) .
C1 C2 1.500(8) .
C2 C7 1.369(8) .
C2 C3 1.385(8) .
C3 C4 1.407(8) .
C4 C5 1.400(8) .
C5 C6 1.380(8) .
C6 C7 1.401(8) .
C8 C9 1.360(9) .
C9 C10 1.360(9) .
C10 C11 1.378(9) .
C11 C12 1.386(9) .
C12 C13 1.484(8) .
C13 C14 1.379(9) .
C14 C15 1.380(10) .
C15 C16 1.363(10) .
C16 C17 1.364(9) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1W O2W 0.85 1.94 2.716(6) 150.7 .
O1W H2W O3W 0.85 2.54 2.747(6) 94.7 6_556
O2W H4W O1W 0.85 2.53 2.716(6) 93.3 .
O2W H4W O4 0.85 2.63 2.713(6) 86.5 .
O2W H4W O5W 0.85 2.32 2.800(7) 115.7 7_565
O2W H3W O7W 0.85 1.85 2.688(7) 170.5 7_565
O3W H6W O1W 0.85 2.15 2.747(6) 126.7 6_656
O3W H5W O6W 0.85 2.12 2.866(7) 146.2 7_566
O4W H7W O3W 0.85 2.81 2.865(7) 85.4 7_565
O4W H8W O5W 0.85 1.92 2.763(7) 170.4 6_656
O5W H9W O1 0.85 2.43 3.054(6) 130.7 .
O5W H10W O2W 0.85 2.39 2.800(7) 110.2 7_566
O6W H11W O3W 0.85 2.54 2.866(7) 104.2 7_565
O6W H12W O5W 0.85 2.17 2.985(7) 159.4 7_565
O6W H11W O7W 0.85 2.78 2.863(7) 86.9 .
O7W H14W O2 0.85 2.68 2.748(6) 85.8 .
O7W H13W O6W 0.85 2.17 2.863(7) 138.9 .
O1 H1A O6 0.82 1.87 2.545(5) 138.5 2_655
O5 H5A O4W 0.82 1.82 2.628(6) 170.6 .
