#------------------------------------------------------------------------------
#$Date: 2016-05-06 04:50:20 +0300 (Fri, 06 May 2016) $
#$Revision: 182737 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/87/7038761.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_7038761
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 H16 Cu N2 O6 P2'
_chemical_formula_weight         469.80
_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
_audit_update_record
;
2016-03-09 deposited with the CCDC.
2016-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                95.020(11)
_cell_angle_beta                 107.860(10)
_cell_angle_gamma                103.549(10)
_cell_formula_units_Z            2
_cell_length_a                   8.539(5)
_cell_length_b                   8.948(5)
_cell_length_c                   12.706(8)
_cell_measurement_reflns_used    8373
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1.71
_cell_volume                     884.9(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 0.971
_diffrn_measured_fraction_theta_max 0.997
_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  0.0287
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7099
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.709
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.455
_exptl_absorpt_correction_T_max  0.816
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_description       block
_exptl_crystal_F_000             478
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0330
_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)+(0.0396P)²+0.5720P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0836
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2658
_reflns_number_total             3110
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt00643d2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7038759--7038764.cif.'
_cod_original_cell_volume        885.0(9)
_cod_database_code               7038761
_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, -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
Cu1 Cu 0.67613(4) 0.67465(4) 0.90288(3) 0.01943(12) Uani 1 1 d . .
O1 O 0.6536(3) 0.6243(2) 0.62081(17) 0.0251(5) Uani 1 1 d . .
O2 O 0.4968(2) 0.3367(2) 0.57547(17) 0.0245(5) Uani 1 1 d . .
H2B H 0.4622 0.3667 0.5157 0.037 Uiso 1 1 calc R U
O3 O 0.6550(2) 0.4672(2) 0.77759(16) 0.0231(5) Uani 1 1 d . .
O4 O 1.4316(2) 0.6020(2) 0.87714(17) 0.0226(5) Uani 1 1 d . .
O5 O 1.4133(2) 0.3145(2) 0.84260(17) 0.0251(5) Uani 1 1 d . .
H5A H 1.4925 0.3548 0.8216 0.038 Uiso 1 1 calc R U
O6 O 1.2516(2) 0.4077(3) 0.95942(17) 0.0259(5) Uani 1 1 d . .
N1 N 0.6422(3) 0.8386(3) 0.8066(2) 0.0207(5) Uani 1 1 d . .
N2 N 0.9220(3) 0.7780(3) 0.9214(2) 0.0223(6) Uani 1 1 d . .
P1 P 0.64994(9) 0.46475(9) 0.65711(6) 0.01790(18) Uani 1 1 d . .
P2 P 1.31851(9) 0.43909(9) 0.86397(6) 0.01770(18) Uani 1 1 d . .
C1 C 0.4911(4) 0.8595(4) 0.7499(3) 0.0286(7) Uani 1 1 d . .
H1A H 0.3929 0.8019 0.7604 0.034 Uiso 1 1 calc R U
C2 C 0.4764(5) 0.9640(4) 0.6762(3) 0.0396(9) Uani 1 1 d . .
H2A H 0.3703 0.9792 0.6396 0.048 Uiso 1 1 calc R U
C3 C 0.6199(5) 1.0453(4) 0.6577(3) 0.0390(9) Uani 1 1 d . .
H3A H 0.6115 1.1131 0.6061 0.047 Uiso 1 1 calc R U
C4 C 0.7768(4) 1.0260(4) 0.7160(3) 0.0331(8) Uani 1 1 d . .
H4A H 0.8758 1.0817 0.7055 0.040 Uiso 1 1 calc R U
C5 C 0.7841(4) 0.9216(3) 0.7908(2) 0.0222(6) Uani 1 1 d . .
C6 C 0.9440(4) 0.8903(3) 0.8588(2) 0.0212(6) Uani 1 1 d . .
C7 C 1.1063(4) 0.9706(4) 0.8615(3) 0.0324(8) Uani 1 1 d . .
H7A H 1.1200 1.0496 0.8194 0.039 Uiso 1 1 calc R U
C8 C 1.2472(4) 0.9307(4) 0.9282(3) 0.0354(8) Uani 1 1 d . .
H8A H 1.3567 0.9824 0.9309 0.042 Uiso 1 1 calc R U
C9 C 1.2241(4) 0.8139(4) 0.9905(3) 0.0344(8) Uani 1 1 d . .
H9A H 1.3172 0.7844 1.0344 0.041 Uiso 1 1 calc R U
C10 C 1.0598(4) 0.7414(4) 0.9865(3) 0.0275(7) Uani 1 1 d . .
H10A H 1.0443 0.6650 1.0303 0.033 Uiso 1 1 calc R U
C11 C 0.9866(4) 0.2196(4) 0.4312(3) 0.0355(8) Uani 1 1 d . .
H11A H 0.8788 0.2080 0.3737 0.053 Uiso 1 1 calc R U
H11B H 1.0033 0.1185 0.4404 0.053 Uiso 1 1 calc R U
H11C H 1.0773 0.2800 0.4100 0.053 Uiso 1 1 calc R U
C12 C 0.9873(4) 0.3016(4) 0.5402(2) 0.0232(7) Uani 1 1 d . .
C13 C 1.1308(4) 0.3328(4) 0.6370(2) 0.0233(7) Uani 1 1 d . .
H13A H 1.2278 0.3059 0.6329 0.028 Uiso 1 1 calc R U
C14 C 1.1325(3) 0.4032(3) 0.7398(2) 0.0188(6) Uani 1 1 d . .
C15 C 0.9860(3) 0.4433(3) 0.7454(2) 0.0199(6) Uani 1 1 d . .
H15A H 0.9851 0.4887 0.8138 0.024 Uiso 1 1 calc R U
C16 C 0.8411(3) 0.4162(3) 0.6496(2) 0.0172(6) Uani 1 1 d . .
C17 C 0.8451(4) 0.3468(3) 0.5481(2) 0.0209(6) Uani 1 1 d . .
H17A H 0.7500 0.3301 0.4837 0.025 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'
Cu Cu 0.3201 1.2651 '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'
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
O6 Cu1 O4 95.88(8) 2_767 1_455
O6 Cu1 N1 156.83(10) 2_767 .
O4 Cu1 N1 91.69(9) 1_455 .
O6 Cu1 N2 90.63(9) 2_767 .
O4 Cu1 N2 171.67(9) 1_455 .
N1 Cu1 N2 80.34(10) . .
O6 Cu1 O3 99.29(9) 2_767 .
O4 Cu1 O3 90.17(8) 1_455 .
N1 Cu1 O3 102.56(10) . .
N2 Cu1 O3 93.91(9) . .
P1 O3 Cu1 127.72(12) . .
P2 O4 Cu1 130.27(12) . 1_655
P2 O6 Cu1 136.20(13) . 2_767
C1 N1 C5 118.9(3) . .
C1 N1 Cu1 125.3(2) . .
C5 N1 Cu1 115.4(2) . .
C10 N2 C6 119.2(3) . .
C10 N2 Cu1 125.9(2) . .
C6 N2 Cu1 114.85(19) . .
O3 P1 O1 112.43(12) . .
O3 P1 O2 111.90(12) . .
O1 P1 O2 111.01(12) . .
O3 P1 C16 106.83(12) . .
O1 P1 C16 107.60(12) . .
O2 P1 C16 106.72(13) . .
O4 P2 O6 115.40(12) . .
O4 P2 O5 110.27(12) . .
O6 P2 O5 109.94(12) . .
O4 P2 C14 109.20(12) . .
O6 P2 C14 106.04(13) . .
O5 P2 C14 105.45(13) . .
N1 C1 C2 122.0(3) . .
C3 C2 C1 119.1(3) . .
C2 C3 C4 119.6(3) . .
C3 C4 C5 118.6(3) . .
N1 C5 C4 121.7(3) . .
N1 C5 C6 114.2(3) . .
C4 C5 C6 124.1(3) . .
N2 C6 C7 121.4(3) . .
N2 C6 C5 114.7(2) . .
C7 C6 C5 123.9(3) . .
C8 C7 C6 118.7(3) . .
C9 C8 C7 119.7(3) . .
C8 C9 C10 118.8(3) . .
N2 C10 C9 122.1(3) . .
C17 C12 C13 118.0(3) . .
C17 C12 C11 121.4(3) . .
C13 C12 C11 120.6(3) . .
C14 C13 C12 121.7(3) . .
C13 C14 C15 118.8(3) . .
C13 C14 P2 120.7(2) . .
C15 C14 P2 120.5(2) . .
C16 C15 C14 121.0(3) . .
C17 C16 C15 118.4(3) . .
C17 C16 P1 120.5(2) . .
C15 C16 P1 121.1(2) . .
C12 C17 C16 122.0(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O6 1.940(2) 2_767
Cu1 O4 1.949(2) 1_455
Cu1 N1 2.007(3) .
Cu1 N2 2.017(3) .
Cu1 O3 2.273(2) .
O1 P1 1.535(2) .
O2 P1 1.535(2) .
O3 P1 1.516(2) .
O4 P2 1.511(2) .
O4 Cu1 1.949(2) 1_655
O5 P2 1.574(2) .
O6 P2 1.512(2) .
O6 Cu1 1.940(2) 2_767
N1 C1 1.336(4) .
N1 C5 1.347(4) .
N2 C10 1.345(4) .
N2 C6 1.350(4) .
P1 C16 1.811(3) .
P2 C14 1.803(3) .
C1 C2 1.380(5) .
C2 C3 1.370(5) .
C3 C4 1.377(5) .
C4 C5 1.388(4) .
C5 C6 1.479(4) .
C6 C7 1.392(4) .
C7 C8 1.386(5) .
C8 C9 1.379(5) .
C9 C10 1.384(4) .
C11 C12 1.508(4) .
C12 C17 1.395(4) .
C12 C13 1.395(4) .
C13 C14 1.394(4) .
C14 C15 1.399(4) .
C15 C16 1.399(4) .
C16 C17 1.395(4) .
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
O2 H2B O1 0.82 1.73 2.528(3) 163.0 2_666
O5 H5A O3 0.82 1.78 2.595(3) 171.8 1_655
C1 H1A O4 0.93 2.44 2.965(4) 115.8 1_455
C3 H3A O2 0.93 2.44 3.175(4) 136.4 1_565
C10 H10A O6 0.93 2.50 2.990(4) 112.8 2_767
