#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:21:14 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180423 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/92/7209224.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_7209224
loop_
_publ_author_name
'Tang, Si-Fu'
'Pan, Xiao-Bo'
'Lv, Xiao-Xia'
'Yan, Shi-Hai'
'Xu, Xian-Rui'
'Li, Liang-Jun'
'Zhao, Xue-Bo'
_publ_section_title
;
 Fabrication of new metal phosphonates from tritopic trisphosphonic acid
 containing methyl groups and auxiliary ligands: syntheses, structures and
 gas adsorption properties
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              1860
_journal_paper_doi               10.1039/c2ce26828k
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C22 H31 N2 Ni O11 P3'
_chemical_formula_weight         651.11
_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                94.0540(10)
_cell_angle_beta                 106.8400(10)
_cell_angle_gamma                93.6490(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9667(6)
_cell_length_b                   10.4207(6)
_cell_length_c                   13.3783(8)
_cell_measurement_reflns_used    3066
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      26.21
_cell_measurement_theta_min      2.14
_cell_volume                     1321.40(14)
_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      273(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_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  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7459
_diffrn_reflns_theta_full        26.21
_diffrn_reflns_theta_max         26.21
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    0.979
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5227
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0412P)²+1.2213P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.1023
_reflns_number_gt                4253
_reflns_number_total             5227
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26828k.txt
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7209224
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
Ni1 Ni 0.34442(4) 0.23373(4) 0.13780(3) 0.01471(11) Uani 1 1 d .
O1W O 0.3570(2) 0.07990(19) 0.02882(17) 0.0211(5) Uani 1 1 d .
H1W H 0.3999 0.0970 -0.0157 0.025 Uiso 1 1 d R
H2W H 0.4006 0.0233 0.0650 0.025 Uiso 1 1 d R
O1 O 0.5302(2) 0.6540(2) 0.56959(17) 0.0190(5) Uani 1 1 d .
O2W O 0.3997(2) 0.37383(19) 0.05344(16) 0.0191(5) Uani 1 1 d .
H3W H 0.4210 0.4486 0.0864 0.023 Uiso 1 1 d R
H4W H 0.4356 0.3664 0.0031 0.023 Uiso 1 1 d R
O2 O 0.5937(2) 0.43306(19) 0.62225(17) 0.0180(5) Uani 1 1 d .
H2A H 0.5555 0.4157 0.5592 0.027 Uiso 1 1 calc R
O3 O 0.6628(2) 0.6167(2) 0.75982(17) 0.0203(5) Uani 1 1 d .
O4 O 0.4645(2) 0.7609(2) 0.26827(17) 0.0207(5) Uani 1 1 d .
H4A H 0.4584 0.6905 0.2912 0.031 Uiso 1 1 calc R
O5 O 0.4790(2) 0.6391(2) 0.10123(17) 0.0197(5) Uani 1 1 d .
O6 O 0.5383(2) 0.88241(19) 0.13846(17) 0.0175(5) Uani 1 1 d .
O7 O 0.7130(2) 0.0408(2) 0.27231(19) 0.0239(5) Uani 1 1 d .
H7C H 0.6482 -0.0021 0.2281 0.036 Uiso 1 1 calc R
O8 O 0.6221(2) 0.1678(2) 0.39902(17) 0.0216(5) Uani 1 1 d .
H8D H 0.5739 0.2271 0.4049 0.032 Uiso 1 1 calc R
O9 O 0.5523(2) 0.2162(2) 0.20915(17) 0.0202(5) Uani 1 1 d .
N1 N 0.2468(3) 0.0937(2) 0.2072(2) 0.0185(6) Uani 1 1 d .
N2 N 0.1327(3) 0.2433(2) 0.0600(2) 0.0188(6) Uani 1 1 d .
P1 P 0.63871(9) 0.58338(7) 0.64556(6) 0.01581(18) Uani 1 1 d .
P2 P 0.54239(8) 0.74992(7) 0.18122(6) 0.01462(18) Uani 1 1 d .
P3 P 0.66595(8) 0.17523(7) 0.29661(7) 0.01668(18) Uani 1 1 d .
C1 C 0.7985(3) 0.5750(3) 0.5051(2) 0.0158(6) Uani 1 1 d .
C2 C 0.7667(3) 0.6673(3) 0.4314(2) 0.0169(6) Uani 1 1 d .
C3 C 0.7538(3) 0.6318(3) 0.3262(2) 0.0142(6) Uani 1 1 d .
C4 C 0.7718(3) 0.5054(3) 0.2927(2) 0.0162(6) Uani 1 1 d .
C5 C 0.8083(3) 0.4150(3) 0.3675(2) 0.0151(6) Uani 1 1 d .
C6 C 0.8222(3) 0.4488(3) 0.4729(2) 0.0152(6) Uani 1 1 d .
C7 C 0.8053(3) 0.6095(3) 0.6179(2) 0.0182(7) Uani 1 1 d .
H7A H 0.8397 0.6998 0.6367 0.022 Uiso 1 1 calc R
H7B H 0.8728 0.5587 0.6620 0.022 Uiso 1 1 calc R
C8 C 0.7508(4) 0.8050(3) 0.4686(3) 0.0226(7) Uani 1 1 d .
H8A H 0.7285 0.8559 0.4098 0.034 Uiso 1 1 calc R
H8B H 0.8373 0.8411 0.5186 0.034 Uiso 1 1 calc R
H8C H 0.6764 0.8052 0.5009 0.034 Uiso 1 1 calc R
C9 C 0.7257(3) 0.7340(3) 0.2480(2) 0.0155(6) Uani 1 1 d .
H9A H 0.7729 0.7138 0.1955 0.019 Uiso 1 1 calc R
H9B H 0.7679 0.8169 0.2849 0.019 Uiso 1 1 calc R
C10 C 0.7593(3) 0.4662(3) 0.1793(2) 0.0195(7) Uani 1 1 d .
H10A H 0.7334 0.5379 0.1386 0.029 Uiso 1 1 calc R
H10B H 0.6886 0.3951 0.1532 0.029 Uiso 1 1 calc R
H10C H 0.8481 0.4407 0.1740 0.029 Uiso 1 1 calc R
C11 C 0.8270(3) 0.2785(3) 0.3298(2) 0.0170(6) Uani 1 1 d .
H11A H 0.8978 0.2430 0.3843 0.020 Uiso 1 1 calc R
H11B H 0.8605 0.2808 0.2687 0.020 Uiso 1 1 calc R
C12 C 0.8687(3) 0.3537(3) 0.5542(2) 0.0186(7) Uani 1 1 d .
H12A H 0.8735 0.3936 0.6222 0.028 Uiso 1 1 calc R
H12B H 0.9599 0.3285 0.5546 0.028 Uiso 1 1 calc R
H12C H 0.8023 0.2788 0.5373 0.028 Uiso 1 1 calc R
C13 C 0.3102(4) 0.0199(3) 0.2817(3) 0.0229(7) Uani 1 1 d .
H13A H 0.4080 0.0267 0.3055 0.027 Uiso 1 1 calc R
C14 C 0.2365(4) -0.0662(3) 0.3249(3) 0.0310(9) Uani 1 1 d .
H14A H 0.2838 -0.1159 0.3768 0.037 Uiso 1 1 calc R
C15 C 0.0931(4) -0.0769(4) 0.2899(3) 0.0399(10) Uani 1 1 d .
H15A H 0.0411 -0.1326 0.3188 0.048 Uiso 1 1 calc R
C16 C 0.0258(4) -0.0038(4) 0.2108(3) 0.0349(9) Uani 1 1 d .
H16A H -0.0718 -0.0120 0.1845 0.042 Uiso 1 1 calc R
C17 C 0.1049(3) 0.0814(3) 0.1712(3) 0.0212(7) Uani 1 1 d .
C18 C 0.0410(4) 0.1658(3) 0.0890(3) 0.0227(7) Uani 1 1 d .
C19 C -0.1025(4) 0.1666(4) 0.0455(3) 0.0353(9) Uani 1 1 d .
H19A H -0.1643 0.1114 0.0664 0.042 Uiso 1 1 calc R
C20 C -0.1539(4) 0.2510(4) -0.0298(3) 0.0432(11) Uani 1 1 d .
H20A H -0.2502 0.2538 -0.0597 0.052 Uiso 1 1 calc R
C21 C -0.0589(4) 0.3303(4) -0.0589(3) 0.0378(10) Uani 1 1 d .
H21A H -0.0901 0.3877 -0.1091 0.045 Uiso 1 1 calc R
C22 C 0.0813(4) 0.3238(3) -0.0134(3) 0.0273(8) Uani 1 1 d .
H22A H 0.1445 0.3775 -0.0341 0.033 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'
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'
Ni Ni 0.3393 1.1124 '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 Ni1 O9 93.10(9) 2_666 .
O3 Ni1 O2W 84.70(8) 2_666 .
O9 Ni1 O2W 89.66(9) . .
O3 Ni1 N2 89.81(10) 2_666 .
O9 Ni1 N2 177.09(10) . .
O2W Ni1 N2 90.79(9) . .
O3 Ni1 N1 95.34(9) 2_666 .
O9 Ni1 N1 101.50(9) . .
O2W Ni1 N1 168.81(10) . .
N2 Ni1 N1 78.03(10) . .
O3 Ni1 O1W 178.20(9) 2_666 .
O9 Ni1 O1W 85.99(9) . .
O2W Ni1 O1W 93.75(8) . .
N2 Ni1 O1W 91.11(9) . .
N1 Ni1 O1W 86.36(9) . .
P1 O3 Ni1 140.76(13) . 2_666
P3 O9 Ni1 150.73(14) . .
C13 N1 C17 118.5(3) . .
C13 N1 Ni1 127.1(2) . .
C17 N1 Ni1 114.4(2) . .
C18 N2 C22 118.1(3) . .
C18 N2 Ni1 116.5(2) . .
C22 N2 Ni1 125.4(2) . .
O3 P1 O1 117.64(12) . .
O3 P1 O2 107.17(12) . .
O1 P1 O2 108.47(12) . .
O3 P1 C7 108.20(14) . .
O1 P1 C7 108.34(14) . .
O2 P1 C7 106.50(13) . .
O5 P2 O6 115.04(12) . .
O5 P2 O4 111.58(12) . .
O6 P2 O4 105.20(12) . .
O5 P2 C9 111.74(13) . .
O6 P2 C9 105.84(13) . .
O4 P2 C9 106.86(13) . .
O9 P3 O7 113.55(13) . .
O9 P3 O8 112.40(13) . .
O7 P3 O8 106.18(12) . .
O9 P3 C11 113.85(13) . .
O7 P3 C11 103.06(13) . .
O8 P3 C11 107.03(14) . .
C2 C1 C6 119.8(3) . .
C2 C1 C7 120.5(3) . .
C6 C1 C7 119.6(3) . .
C3 C2 C1 119.8(3) . .
C3 C2 C8 121.0(3) . .
C1 C2 C8 119.2(3) . .
C2 C3 C4 120.8(3) . .
C2 C3 C9 119.3(3) . .
C4 C3 C9 119.9(3) . .
C3 C4 C5 119.0(3) . .
C3 C4 C10 121.3(3) . .
C5 C4 C10 119.7(3) . .
C6 C5 C4 120.9(3) . .
C6 C5 C11 120.7(3) . .
C4 C5 C11 118.3(3) . .
C5 C6 C1 119.6(3) . .
C5 C6 C12 120.9(3) . .
C1 C6 C12 119.4(3) . .
C1 C7 P1 114.3(2) . .
C3 C9 P2 115.8(2) . .
C5 C11 P3 112.2(2) . .
N1 C13 C14 122.8(3) . .
C15 C14 C13 118.8(3) . .
C14 C15 C16 119.2(3) . .
C17 C16 C15 119.5(3) . .
N1 C17 C16 121.2(3) . .
N1 C17 C18 115.9(3) . .
C16 C17 C18 122.8(3) . .
N2 C18 C19 121.9(3) . .
N2 C18 C17 115.1(3) . .
C19 C18 C17 123.0(3) . .
C18 C19 C20 119.3(3) . .
C21 C20 C19 118.4(4) . .
C22 C21 C20 119.2(3) . .
N2 C22 C21 123.1(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O3 2.020(2) 2_666
Ni1 O9 2.040(2) .
Ni1 O2W 2.049(2) .
Ni1 N2 2.077(3) .
Ni1 N1 2.115(3) .
Ni1 O1W 2.124(2) .
O1 P1 1.521(2) .
O2 P1 1.585(2) .
O3 P1 1.489(2) .
O3 Ni1 2.020(2) 2_666
O4 P2 1.578(2) .
O5 P2 1.490(2) .
O6 P2 1.530(2) .
O7 P3 1.547(2) .
O8 P3 1.559(2) .
O9 P3 1.483(2) .
N1 C13 1.338(4) .
N1 C17 1.350(4) .
N2 C18 1.340(4) .
N2 C22 1.346(4) .
P1 C7 1.811(3) .
P2 C9 1.810(3) .
P3 C11 1.798(3) .
C1 C2 1.410(4) .
C1 C6 1.411(4) .
C1 C7 1.508(4) .
C2 C3 1.396(4) .
C2 C8 1.519(4) .
C3 C4 1.401(4) .
C3 C9 1.527(4) .
C4 C5 1.410(4) .
C4 C10 1.510(4) .
C5 C6 1.393(4) .
C5 C11 1.516(4) .
C6 C12 1.516(4) .
C13 C14 1.383(5) .
C14 C15 1.363(5) .
C15 C16 1.385(5) .
C16 C17 1.382(5) .
C17 C18 1.480(4) .
C18 C19 1.380(5) .
C19 C20 1.391(5) .
C20 C21 1.375(5) .
C21 C22 1.361(5) .
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 O6 0.85 1.93 2.770(3) 167.8 2_665
O2W H3W O5 0.85 2.01 2.802(3) 154.4 .
O2W H4W O5 0.85 1.83 2.681(3) 175.9 2_665
O2 H2A O1 0.82 1.77 2.574(3) 168.4 2_666
O7 H7C O6 0.82 1.72 2.524(3) 167.4 1_545
O8 H8D O1 0.82 1.74 2.558(3) 173.5 2_666
O1W H2W O6 0.85 2.16 3.003(3) 169.0 1_545
