#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:25:00 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180504 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/73/7217361.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_7217361
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 H26 Co O14 P2'
_chemical_formula_weight         467.16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.523(4)
_cell_angle_beta                 95.780(4)
_cell_angle_gamma                91.060(4)
_cell_formula_units_Z            2
_cell_length_a                   6.8159(18)
_cell_length_b                   9.734(3)
_cell_length_c                   13.799(4)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.59
_cell_measurement_theta_min      2.11
_cell_volume                     904.5(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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.0502
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8529
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    1.192
_exptl_absorpt_correction_T_max  0.888
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             486
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0551P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1208
_reflns_number_gt                3180
_reflns_number_total             4065
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7216042
_cod_data_source_file            c4ce00375f2.cif
_cod_data_source_block           2
_cod_original_cell_volume        904.6(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7217361
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Co1 Co 0.75923(6) 0.68972(4) 0.07281(3) 0.01885(14) Uani 1 1 d .
O1 O 0.8597(3) 0.4400(2) 0.28955(16) 0.0251(5) Uani 1 1 d .
O1W O 0.9602(3) 0.6327(2) 0.17848(17) 0.0312(6) Uani 1 1 d .
H1W H 0.9349 0.5738 0.2169 0.037 Uiso 1 1 d R
H2W H 1.0630 0.6812 0.2013 0.037 Uiso 1 1 d R
O2 O 0.7030(3) 0.2134(2) 0.30297(17) 0.0280(5) Uani 1 1 d .
H2A H 0.6120 0.1672 0.2708 0.042 Uiso 1 1 calc R
O2W O 0.7539(3) 0.4902(2) 0.00500(17) 0.0330(6) Uani 1 1 d .
H3W H 0.8428 0.4301 0.0046 0.040 Uiso 1 1 d R
H4W H 0.6416 0.4576 -0.0207 0.040 Uiso 1 1 d R
O3W O 0.9882(3) 0.7337(2) -0.01487(16) 0.0269(5) Uani 1 1 d .
H5W H 1.0737 0.7997 -0.0023 0.032 Uiso 1 1 d R
H6W H 0.9537 0.7423 -0.0747 0.032 Uiso 1 1 d R
O3 O 0.5024(3) 0.3890(2) 0.21776(15) 0.0239(5) Uani 1 1 d .
O4W O 0.5160(3) 0.6309(2) 0.14278(15) 0.0235(5) Uani 1 1 d .
H7W H 0.5194 0.5431 0.1368 0.028 Uiso 1 1 d R
H8W H 0.4413 0.6836 0.1748 0.028 Uiso 1 1 d R
O4 O 0.1187(3) 1.0147(2) 0.26531(16) 0.0233(5) Uani 1 1 d .
H4A H 0.1350 1.0922 0.2492 0.035 Uiso 1 1 calc R
O5W O 0.7781(3) 0.9012(2) 0.13598(15) 0.0244(5) Uani 1 1 d .
H9W H 0.8873 0.9245 0.1698 0.029 Uiso 1 1 d R
H10W H 0.6783 0.9314 0.1631 0.029 Uiso 1 1 d R
O5 O 0.2820(3) 0.7897(2) 0.24296(16) 0.0237(5) Uani 1 1 d .
O6W O 0.5597(3) 0.7548(2) -0.03703(16) 0.0284(5) Uani 1 1 d .
H11W H 0.5283 0.7121 -0.0939 0.034 Uiso 1 1 d R
H12W H 0.4663 0.8059 -0.0201 0.034 Uiso 1 1 d R
O6 O 0.4618(3) 1.0084(2) 0.21228(15) 0.0204(5) Uani 1 1 d .
O7W O 1.2697(3) 0.9376(2) 0.02269(17) 0.0312(5) Uani 1 1 d .
H13W H 1.2548 1.0034 -0.0127 0.037 Uiso 1 1 d R
H14W H 1.3256 0.9552 0.0808 0.037 Uiso 1 1 d R
O8W O 0.1277(3) 1.2680(2) 0.21453(17) 0.0283(5) Uani 1 1 d .
H15W H 0.2406 1.3072 0.2164 0.034 Uiso 1 1 d R
H16W H 0.0407 1.3174 0.2402 0.034 Uiso 1 1 d R
P1 P 0.66399(11) 0.37193(8) 0.29917(6) 0.01786(18) Uani 1 1 d .
P2 P 0.32357(11) 0.94062(8) 0.27407(6) 0.01771(18) Uani 1 1 d .
C1 C 0.8558(5) 0.3379(4) 0.5174(3) 0.0314(8) Uani 1 1 d .
H1A H 0.8985 0.3382 0.5859 0.047 Uiso 1 1 calc R
H1B H 0.9583 0.3779 0.4857 0.047 Uiso 1 1 calc R
H1C H 0.8273 0.2445 0.4882 0.047 Uiso 1 1 calc R
C2 C 0.6726(4) 0.4214(3) 0.5056(2) 0.0207(6) Uani 1 1 d .
C3 C 0.5742(4) 0.4396(3) 0.4142(2) 0.0187(6) Uani 1 1 d .
C4 C 0.4043(5) 0.5171(3) 0.4105(2) 0.0230(7) Uani 1 1 d .
H4B H 0.3392 0.5282 0.3495 0.028 Uiso 1 1 calc R
C5 C 0.7191(5) 0.8173(4) 0.3702(2) 0.0331(8) Uani 1 1 d .
H5A H 0.8303 0.7860 0.4093 0.050 Uiso 1 1 calc R
H5B H 0.7646 0.8666 0.3199 0.050 Uiso 1 1 calc R
H5C H 0.6378 0.7392 0.3406 0.050 Uiso 1 1 calc R
C6 C 0.6007(4) 0.9119(3) 0.4345(2) 0.0213(6) Uani 1 1 d .
C7 C 0.4248(4) 0.9717(3) 0.4011(2) 0.0188(6) Uani 1 1 d .
C8 C 0.3287(4) 1.0578(3) 0.4669(2) 0.0226(7) Uani 1 1 d .
H8A H 0.2121 1.0971 0.4442 0.027 Uiso 1 1 calc R
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'
Co Co 0.3494 0.9721 '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 Co1 O2W 88.49(9) . .
O1W Co1 O6W 177.74(8) . .
O2W Co1 O6W 92.82(9) . .
O1W Co1 O4W 93.78(9) . .
O2W Co1 O4W 87.22(9) . .
O6W Co1 O4W 88.12(9) . .
O1W Co1 O3W 90.90(9) . .
O2W Co1 O3W 87.11(9) . .
O6W Co1 O3W 87.33(9) . .
O4W Co1 O3W 172.55(8) . .
O1W Co1 O5W 92.27(9) . .
O2W Co1 O5W 175.97(9) . .
O6W Co1 O5W 86.30(9) . .
O4W Co1 O5W 96.67(8) . .
O3W Co1 O5W 88.92(8) . .
O1 P1 O3 115.38(12) . .
O1 P1 O2 106.46(12) . .
O3 P1 O2 109.58(12) . .
O1 P1 C3 109.91(13) . .
O3 P1 C3 107.38(13) . .
O2 P1 C3 107.93(13) . .
O5 P2 O6 114.24(12) . .
O5 P2 O4 107.03(12) . .
O6 P2 O4 108.43(12) . .
O5 P2 C7 111.35(13) . .
O6 P2 C7 108.38(12) . .
O4 P2 C7 107.13(13) . .
C4 C2 C3 118.0(3) 2_666 .
C4 C2 C1 118.9(3) 2_666 .
C3 C2 C1 123.1(3) . .
C4 C3 C2 119.1(3) . .
C4 C3 P1 118.2(2) . .
C2 C3 P1 122.7(2) . .
C3 C4 C2 122.9(3) . 2_666
C8 C6 C7 118.0(3) 2_676 .
C8 C6 C5 117.8(3) 2_676 .
C7 C6 C5 124.1(3) . .
C8 C7 C6 119.1(3) . .
C8 C7 P2 119.7(2) . .
C6 C7 P2 121.3(2) . .
C7 C8 C6 122.9(3) . 2_676
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O1W 2.030(2) .
Co1 O2W 2.056(2) .
Co1 O6W 2.094(2) .
Co1 O4W 2.102(2) .
Co1 O3W 2.135(2) .
Co1 O5W 2.139(2) .
O1 P1 1.503(2) .
O2 P1 1.576(2) .
O3 P1 1.517(2) .
O4 P2 1.583(2) .
O5 P2 1.497(2) .
O6 P2 1.522(2) .
P1 C3 1.818(3) .
P2 C7 1.808(3) .
C1 C2 1.507(4) .
C2 C4 1.396(4) 2_666
C2 C3 1.399(4) .
C3 C4 1.393(4) .
C4 C2 1.396(4) 2_666
C5 C6 1.507(4) .
C6 C8 1.394(4) 2_676
C6 C7 1.401(4) .
C7 C8 1.387(4) .
C8 C6 1.394(4) 2_676
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 H2A O6 0.82 1.89 2.674(3) 158.8 1_545
O1W H2W O5 0.85 1.82 2.667(3) 176.4 1_655
O2W H3W O3W 0.85 1.99 2.832(3) 168.5 2_765
O2W H4W O4W 0.85 2.00 2.748(3) 146.0 2_665
O3W H6W O8W 0.85 1.94 2.787(3) 171.4 2_675
O3W H5W O7W 0.85 1.86 2.704(3) 177.0 .
O4W H7W O2W 0.85 2.55 2.748(3) 94.3 2_665
O4W H7W O3 0.85 1.98 2.681(3) 139.4 .
O5W H9W O4 0.85 2.06 2.901(3) 167.9 1_655
O6W H11W O3 0.85 1.86 2.707(3) 171.6 2_665
O6W H12W O7W 0.85 1.96 2.806(3) 174.7 1_455
O7W H13W O5W 0.85 2.02 2.832(3) 158.4 2_775
O7W H14W O6 0.85 1.96 2.811(3) 175.9 1_655
O8W H15W O3 0.85 1.94 2.787(3) 177.4 1_565
C1 H1B O1 0.96 2.86 3.406(4) 117.3 .
C1 H1C O2 0.96 2.59 3.135(4) 116.0 .
C5 H5C O5 0.96 2.73 3.293(4) 117.8 .
C5 H5B O6 0.96 2.89 3.400(4) 114.6 .
