#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:07:42 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180491 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/60/7216045.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_7216045
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 Cu O8 P2'
_chemical_formula_weight         363.67
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                75.102(5)
_cell_angle_beta                 84.496(10)
_cell_angle_gamma                76.610(3)
_cell_formula_units_Z            1
_cell_length_a                   5.1671(10)
_cell_length_b                   6.3007(12)
_cell_length_c                   10.029(3)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.998
_cell_measurement_theta_min      2.103
_cell_volume                     306.72(12)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.986
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2400
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.103
_exptl_absorpt_coefficient_mu    2.074
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.969
_exptl_crystal_description       plate
_exptl_crystal_F_000             185
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         1063
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0379
_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)+(0.0455P)²+0.4350P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.0998
_reflns_Friedel_coverage         0.000
_reflns_number_gt                893
_reflns_number_total             1063
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4ce00375f2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7216041--7216048.cif.'
_cod_original_cell_volume        306.73(12)
_cod_database_code               7216045
#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'
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
Cu1 Cu 1.0000 1.0000 0.0000 0.0209(3) Uani 1 2 d S . P
O1 O 0.5444(6) 0.6897(5) 0.1974(3) 0.0288(7) Uani 1 1 d . . .
H1A H 0.4123 0.6499 0.1818 0.043 Uiso 1 1 calc R U .
O1W O 1.0648(7) 0.5373(6) 0.1386(4) 0.0499(10) Uani 1 1 d . . .
H1W H 1.0654 0.5110 0.2261 0.060 Uiso 1 1 d R U .
H2W H 1.0827 0.4214 0.1072 0.060 Uiso 1 1 d R U .
O2 O 0.6739(5) 1.0653(5) 0.1060(3) 0.0228(6) Uani 1 1 d . . .
O3 O 0.1876(5) 1.0385(5) 0.1486(3) 0.0248(7) Uani 1 1 d . . .
P1 P 0.47081(19) 0.94880(17) 0.19256(10) 0.0169(3) Uani 1 1 d . . .
C1 C 0.4793(7) 0.9737(7) 0.3679(4) 0.0163(8) Uani 1 1 d . . .
C2 C 0.6315(8) 1.1163(7) 0.3907(4) 0.0185(8) Uani 1 1 d . . .
H2A H 0.7212 1.1937 0.3159 0.022 Uiso 1 1 calc R U .
C3 C 0.3462(8) 0.8534(6) 0.4791(4) 0.0180(8) Uani 1 1 d . . .
C4 C 0.1792(9) 0.6951(7) 0.4638(4) 0.0261(10) Uani 1 1 d . . .
H4A H 0.2933 0.5593 0.4483 0.039 Uiso 1 1 calc R U .
H4B H 0.0665 0.7650 0.3869 0.039 Uiso 1 1 calc R U .
H4C H 0.0714 0.6602 0.5465 0.039 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'
Cu Cu 0.3201 1.2651 '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'
H H 0.0000 0.0000 '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
O2 Cu1 O2 180.0 2_775 .
O2 Cu1 O3 87.99(11) 2_775 2_675
O2 Cu1 O3 92.01(11) . 2_675
O2 Cu1 O3 92.01(11) 2_775 1_655
O2 Cu1 O3 87.99(11) . 1_655
O3 Cu1 O3 180.0 2_675 1_655
O2 Cu1 O1W 90.45(11) 2_775 .
O2 Cu1 O1W 89.55(11) . .
O3 Cu1 O1W 92.06(12) 2_675 .
O3 Cu1 O1W 87.94(12) 1_655 .
P1 O1 H1A 109.5 . .
Cu1 O1W H1W 114.4 . .
Cu1 O1W H2W 130.8 . .
H1W O1W H2W 114.8 . .
P1 O2 Cu1 140.3(2) . .
P1 O3 Cu1 131.79(18) . 1_455
O2 P1 O3 115.76(17) . .
O2 P1 O1 110.47(17) . .
O3 P1 O1 107.86(17) . .
O2 P1 C1 108.23(16) . .
O3 P1 C1 107.24(16) . .
O1 P1 C1 106.89(17) . .
C2 C1 C3 119.7(3) . .
C2 C1 P1 117.4(3) . .
C3 C1 P1 122.8(3) . .
C3 C2 C1 122.3(4) 2_676 .
C3 C2 H2A 118.9 2_676 .
C1 C2 H2A 118.9 . .
C2 C3 C1 118.0(4) 2_676 .
C2 C3 C4 118.9(4) 2_676 .
C1 C3 C4 123.2(3) . .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O2 1.924(3) 2_775
Cu1 O2 1.924(3) .
Cu1 O3 1.948(3) 2_675
Cu1 O3 1.948(3) 1_655
Cu1 O1W 2.846(4) .
O1 P1 1.577(3) .
O1 H1A 0.8200 .
O1W H1W 0.8500 .
O1W H2W 0.8500 .
O2 P1 1.499(3) .
O3 P1 1.506(3) .
O3 Cu1 1.948(3) 1_455
P1 C1 1.811(4) .
C1 C2 1.395(5) .
C1 C3 1.397(5) .
C2 C3 1.387(5) 2_676
C2 H2A 0.9300 .
C3 C2 1.387(5) 2_676
C3 C4 1.505(5) .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
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 O1W 0.82 2.19 3.014(5) 178.7 1_455
O1W H2W O1W 0.85 2.58 3.094(7) 119.9 2_765
O1W H2W O3 0.85 2.28 3.035(5) 147.8 1_645
C4 H4A O1 0.96 2.74 3.123(5) 104.7 .
C4 H4B O3 0.96 2.68 3.343(5) 126.9 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
Cu1 O2 P1 O3 -124.0(3) . .
Cu1 O2 P1 O1 -1.0(3) . .
Cu1 O2 P1 C1 115.7(3) . .
Cu1 O3 P1 O2 77.5(3) 1_455 .
Cu1 O3 P1 O1 -46.8(3) 1_455 .
Cu1 O3 P1 C1 -161.6(2) 1_455 .
O2 P1 C1 C2 9.1(4) . .
O3 P1 C1 C2 -116.4(3) . .
O1 P1 C1 C2 128.1(3) . .
O2 P1 C1 C3 -169.4(3) . .
O3 P1 C1 C3 65.1(4) . .
O1 P1 C1 C3 -50.4(4) . .
C3 C1 C2 C3 -0.9(6) . 2_676
P1 C1 C2 C3 -179.5(3) . 2_676
C2 C1 C3 C2 0.9(6) . 2_676
P1 C1 C3 C2 179.4(3) . 2_676
C2 C1 C3 C4 -179.6(4) . .
P1 C1 C3 C4 -1.2(6) . .
