#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:07:42 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180491 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/60/7216047.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_7216047
loop_
_publ_author_name
'Tang, Si-Fu'
'Li, Liang-Jun'
'Lv, Xiao-Xia'
'Wang, Chao'
'Zhao, Xue-Bo'
_publ_section_title
;
 Tuning the structure of metal phosphonates using uncoordinating methyl
 group: syntheses, structures and properties of a series of metal
 diphosphonates
;
_journal_issue                   30
_journal_name_full               CrystEngComm
_journal_page_first              7043
_journal_paper_doi               10.1039/C4CE00375F
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C8 H14 Cd O8 P2'
_chemical_formula_weight         412.53
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90.463(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.781(4)
_cell_length_b                   6.7881(15)
_cell_length_c                   9.4449(19)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.991
_cell_measurement_theta_min      2.059
_cell_volume                     1268.2(5)
_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    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.984
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3165
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.991
_diffrn_reflns_theta_min         2.059
_exptl_absorpt_coefficient_mu    2.006
_exptl_absorpt_correction_T_max  0.818
_exptl_absorpt_correction_T_min  0.624
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.161
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       0.0015(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         1097
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0458P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0849
_reflns_Friedel_coverage         0.000
_reflns_number_gt                991
_reflns_number_total             1097
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4ce00375f2.cif
_cod_data_source_block           b
_cod_depositor_comments
'Adding full bibliography for 7216041--7216048.cif.'
_cod_database_code               7216047
#BEGIN Tags that were not found in dictionaries:
_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
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
_atom_site_refinement_flags_occupancy
Cd1 Cd 0.5000 0.20994(6) 0.2500 0.0173(2) Uani 1 2 d S T P
O1 O 0.60405(15) -0.1323(4) 0.4419(3) 0.0215(7) Uani 1 1 d . . .
H1A H 0.5982 -0.1087 0.3575 0.032 Uiso 1 1 calc R U .
O1W O 0.56656(19) 0.4497(5) 0.1438(5) 0.0435(10) Uani 1 1 d . . .
H1W H 0.5893 0.5354 0.1893 0.052 Uiso 1 1 d R U .
H2W H 0.5740 0.4177 0.0583 0.052 Uiso 1 1 d R U .
O2 O 0.58371(15) 0.0077(5) 0.6786(3) 0.0200(7) Uani 1 1 d . . .
O3 O 0.55335(16) 0.2124(4) 0.4610(3) 0.0196(7) Uani 1 1 d . . .
P1 P 0.60120(5) 0.06658(16) 0.52898(12) 0.0153(3) Uani 1 1 d . . .
C1 C 0.6856(2) 0.1674(6) 0.5206(4) 0.0145(9) Uani 1 1 d . . .
C2 C 0.6942(2) 0.3483(6) 0.4497(5) 0.0179(9) Uani 1 1 d . . .
H2A H 0.6561 0.4142 0.4158 0.022 Uiso 1 1 calc R U .
C3 C 0.7576(2) 0.4320(6) 0.4285(5) 0.0165(9) Uani 1 1 d . . .
C4 C 0.7608(2) 0.6191(7) 0.3427(5) 0.0245(10) Uani 1 1 d . . .
H4A H 0.7704 0.5875 0.2459 0.037 Uiso 1 1 calc R U .
H4B H 0.7959 0.7025 0.3801 0.037 Uiso 1 1 calc R U .
H4C H 0.7182 0.6863 0.3476 0.037 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'
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
O3 Cd1 O3 179.14(14) 2_655 .
O3 Cd1 O2 94.49(11) 2_655 6
O3 Cd1 O2 86.06(10) . 6
O3 Cd1 O2 86.06(11) 2_655 5_656
O3 Cd1 O2 94.49(11) . 5_656
O2 Cd1 O2 101.03(16) 6 5_656
O3 Cd1 O1W 82.87(13) 2_655 .
O3 Cd1 O1W 96.52(13) . .
O2 Cd1 O1W 84.98(13) 6 .
O2 Cd1 O1W 167.80(13) 5_656 .
O3 Cd1 O1W 96.52(13) 2_655 2_655
O3 Cd1 O1W 82.87(13) . 2_655
O2 Cd1 O1W 167.80(13) 6 2_655
O2 Cd1 O1W 84.98(13) 5_656 2_655
O1W Cd1 O1W 91.2(2) . 2_655
P1 O2 Cd1 127.48(17) . 5_656
P1 O3 Cd1 131.35(18) . .
O3 P1 O2 115.07(18) . .
O3 P1 O1 111.30(18) . .
O2 P1 O1 105.66(17) . .
O3 P1 C1 108.02(19) . .
O2 P1 C1 111.07(19) . .
O1 P1 C1 105.30(18) . .
C3 C1 C2 119.0(4) 7_656 .
C3 C1 P1 123.0(3) 7_656 .
C2 C1 P1 117.8(3) . .
C3 C2 C1 122.4(4) . .
C2 C3 C1 118.6(4) . 7_656
C2 C3 C4 117.6(4) . .
C1 C3 C4 123.7(4) 7_656 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 O3 2.248(3) 2_655
Cd1 O3 2.248(3) .
Cd1 O2 2.323(3) 6
Cd1 O2 2.323(3) 5_656
Cd1 O1W 2.326(3) .
Cd1 O1W 2.326(3) 2_655
O1 P1 1.582(3) .
O2 P1 1.512(3) .
O2 Cd1 2.323(3) 5_656
O3 P1 1.509(3) .
P1 C1 1.806(4) .
C1 C3 1.394(6) 7_656
C1 C2 1.410(6) .
C2 C3 1.393(6) .
C3 C1 1.394(6) 7_656
C3 C4 1.508(6) .
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
O1 H1A O2 0.82 1.84 2.654(4) 169.3 6
O1W H2W O3 0.85 2.88 3.027(5) 91.5 2_655
C4 H4B O1 0.96 2.63 3.347(6) 131.7 7_656
C4 H4B O2 0.96 2.84 3.202(5) 103.7 7_656
O1W H2W O1 0.85 2.31 2.976(5) 135.6 6
O1W H2W O3 0.85 2.70 2.882(5) 93.4 6_565
