#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:28:31 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180507 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/76/7217604.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_7217604
loop_
_publ_author_name
'Tang, Si-Fu'
'Li, Liang-Jun'
'Wang, Chao'
'Zhao, Xue-Bo'
_publ_section_title
;
 Investigation of the structure variation of metal diphosphonates with the
 changing of N-donor auxiliary ligands and their properties
;
_journal_issue                   38
_journal_name_full               CrystEngComm
_journal_page_first              9104
_journal_paper_doi               10.1039/C4CE01266F
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C20 H28 N2 Ni O10 P2'
_chemical_formula_weight         577.09
_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                105.480(3)
_cell_angle_beta                 109.935(2)
_cell_angle_gamma                101.391(4)
_cell_formula_units_Z            2
_cell_length_a                   10.3161(14)
_cell_length_b                   11.508(3)
_cell_length_c                   12.0717(16)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1.93
_cell_volume                     1230.8(4)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0573
_diffrn_reflns_av_sigmaI/netI    0.0861
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9768
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.975
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.9
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0497P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1115
_reflns_number_gt                2958
_reflns_number_total             4325
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce01266f2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 7217600--7217608.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7217604
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 -0.15986(6) -0.25343(5) -0.00228(5) 0.02119(17) Uani 1 1 d .
O1W O -0.1763(3) -0.4293(2) 0.0207(2) 0.0273(7) Uani 1 1 d .
H1W H -0.2109 -0.4397 0.0732 0.033 Uiso 1 1 d R
H2W H -0.1502 -0.4858 -0.0197 0.033 Uiso 1 1 d R
O1 O -0.3806(3) -0.2341(3) 0.2588(3) 0.0391(8) Uani 1 1 d .
H1B H -0.4324 -0.3085 0.2299 0.059 Uiso 1 1 calc R
O2W O -0.1409(3) -0.0717(3) -0.0141(3) 0.0380(8) Uani 1 1 d .
H3W H -0.1439 -0.0207 0.0499 0.046 Uiso 1 1 d R
H4W H -0.1309 -0.0521 -0.0744 0.046 Uiso 1 1 d R
O2 O -0.1968(3) -0.3489(2) 0.2483(2) 0.0266(7) Uani 1 1 d .
O3 O -0.2372(3) -0.1949(3) 0.1335(2) 0.0267(7) Uani 1 1 d .
O3W O -0.5409(4) -0.1914(4) -0.0051(4) 0.0770(13) Uani 1 1 d .
H5W H -0.6160 -0.2256 0.0036 0.092 Uiso 1 1 d R
H6W H -0.5545 -0.2619 -0.0600 0.092 Uiso 1 1 d R
O4 O -0.4346(3) -0.5486(2) -0.1782(2) 0.0259(7) Uani 1 1 d .
O4W O -0.3856(4) -0.0214(4) -0.0951(4) 0.0786(13) Uani 1 1 d .
H7W H -0.3828 0.0543 -0.0603 0.094 Uiso 1 1 d R
H8W H -0.4432 -0.0785 -0.0864 0.094 Uiso 1 1 d R
O5 O -0.6282(3) -0.4397(3) -0.2183(3) 0.0311(7) Uani 1 1 d .
H5B H -0.6755 -0.5109 -0.2283 0.047 Uiso 1 1 calc R
O6 O -0.3700(3) -0.3110(2) -0.1345(2) 0.0250(7) Uani 1 1 d .
N1 N 0.0550(4) -0.1795(3) 0.1387(3) 0.0289(9) Uani 1 1 d .
N2 N -0.1055(4) -0.3189(3) -0.1566(3) 0.0251(8) Uani 1 1 d .
P1 P -0.23360(11) -0.22825(10) 0.24659(10) 0.0229(3) Uani 1 1 d .
P2 P -0.47482(11) -0.44142(10) -0.21678(10) 0.0221(3) Uani 1 1 d .
C1 C 0.0039(5) -0.1215(4) 0.4764(4) 0.0265(10) Uani 1 1 d .
H1A H 0.0060 -0.2046 0.4595 0.032 Uiso 1 1 calc R
C2 C -0.1050(4) -0.0965(4) 0.3885(4) 0.0226(9) Uani 1 1 d .
C3 C -0.1092(5) 0.0273(4) 0.4120(4) 0.0266(10) Uani 1 1 d .
C4 C -0.2219(5) 0.0631(4) 0.3198(4) 0.0413(13) Uani 1 1 d .
H4A H -0.1997 0.1539 0.3494 0.062 Uiso 1 1 calc R
H4B H -0.3167 0.0243 0.3137 0.062 Uiso 1 1 calc R
H4C H -0.2206 0.0337 0.2380 0.062 Uiso 1 1 calc R
C5 C -0.4556(4) -0.5741(4) -0.4340(4) 0.0255(10) Uani 1 1 d .
H5A H -0.4252 -0.6247 -0.3884 0.031 Uiso 1 1 calc R
C6 C -0.4941(4) -0.4735(4) -0.3777(4) 0.0226(9) Uani 1 1 d .
C7 C -0.5403(4) -0.3958(4) -0.4453(4) 0.0265(10) Uani 1 1 d .
C8 C -0.5859(6) -0.2843(4) -0.3930(4) 0.0435(13) Uani 1 1 d .
H8A H -0.5063 -0.2238 -0.3169 0.065 Uiso 1 1 calc R
H8B H -0.6673 -0.3134 -0.3747 0.065 Uiso 1 1 calc R
H8C H -0.6130 -0.2446 -0.4542 0.065 Uiso 1 1 calc R
C9 C 0.1503(5) -0.2425(5) 0.1455(4) 0.0451(13) Uani 1 1 d .
H9A H 0.1227 -0.3202 0.0809 0.054 Uiso 1 1 calc R
C10 C 0.0988(5) -0.0673(4) 0.2339(4) 0.0300(11) Uani 1 1 d .
H10A H 0.0351 -0.0201 0.2318 0.036 Uiso 1 1 calc R
C11 C 0.2874(5) -0.2005(5) 0.2418(4) 0.0433(13) Uani 1 1 d .
H11A H 0.3496 -0.2487 0.2400 0.052 Uiso 1 1 calc R
C12 C 0.2343(5) -0.0190(4) 0.3347(4) 0.0340(11) Uani 1 1 d .
H12A H 0.2598 0.0589 0.3984 0.041 Uiso 1 1 calc R
C13 C 0.3325(5) -0.0871(4) 0.3406(4) 0.0301(11) Uani 1 1 d .
C14 C 0.4764(5) -0.0458(4) 0.4454(4) 0.0342(11) Uani 1 1 d .
H14A H 0.5404 -0.0891 0.4329 0.041 Uiso 1 1 calc R
C15 C -0.0513(5) -0.4150(4) -0.1755(4) 0.0346(11) Uani 1 1 d .
H15A H -0.0273 -0.4496 -0.1127 0.042 Uiso 1 1 calc R
C16 C -0.1438(5) -0.2751(4) -0.2513(4) 0.0310(11) Uani 1 1 d .
H16A H -0.1851 -0.2102 -0.2429 0.037 Uiso 1 1 calc R
C17 C -0.0285(5) -0.4664(4) -0.2815(4) 0.0383(12) Uani 1 1 d .
H17A H 0.0104 -0.5329 -0.2887 0.046 Uiso 1 1 calc R
C18 C -0.1252(5) -0.3213(4) -0.3595(4) 0.0343(11) Uani 1 1 d .
H18A H -0.1539 -0.2874 -0.4223 0.041 Uiso 1 1 calc R
C19 C -0.0640(5) -0.4179(4) -0.3772(4) 0.0302(11) Uani 1 1 d .
C20 C -0.0408(5) -0.4644(4) -0.4916(4) 0.0313(11) Uani 1 1 d .
H20A H -0.0883 -0.4414 -0.5589 0.038 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
O6 Ni1 O3 87.21(11) . .
O6 Ni1 O1W 94.31(11) . .
O3 Ni1 O1W 90.84(11) . .
O6 Ni1 N1 175.40(12) . .
O3 Ni1 N1 90.27(12) . .
O1W Ni1 N1 89.57(12) . .
O6 Ni1 O2W 87.27(11) . .
O3 Ni1 O2W 86.26(11) . .
O1W Ni1 O2W 176.63(11) . .
N1 Ni1 O2W 88.73(12) . .
O6 Ni1 N2 86.23(12) . .
O3 Ni1 N2 173.43(12) . .
O1W Ni1 N2 89.98(12) . .
N1 Ni1 N2 96.26(13) . .
O2W Ni1 N2 93.10(12) . .
P1 O3 Ni1 133.81(17) . .
P2 O6 Ni1 130.80(17) . .
C9 N1 C10 116.1(4) . .
C9 N1 Ni1 123.3(3) . .
C10 N1 Ni1 120.4(3) . .
C15 N2 C16 115.9(4) . .
C15 N2 Ni1 124.0(3) . .
C16 N2 Ni1 119.6(3) . .
O3 P1 O2 114.55(16) . .
O3 P1 O1 109.88(17) . .
O2 P1 O1 110.85(17) . .
O3 P1 C2 108.90(17) . .
O2 P1 C2 109.67(18) . .
O1 P1 C2 102.27(18) . .
O6 P2 O4 115.40(16) . .
O6 P2 O5 106.97(16) . .
O4 P2 O5 110.35(16) . .
O6 P2 C6 109.46(17) . .
O4 P2 C6 107.81(17) . .
O5 P2 C6 106.50(17) . .
C3 C1 C2 122.7(4) 2_556 .
C3 C2 C1 119.4(4) . .
C3 C2 P1 122.8(3) . .
C1 C2 P1 117.8(3) . .
C1 C3 C2 117.9(4) 2_556 .
C1 C3 C4 119.4(4) 2_556 .
C2 C3 C4 122.7(4) . .
C6 C5 C7 123.8(4) . 2_444
C5 C6 C7 118.9(4) . .
C5 C6 P2 118.8(3) . .
C7 C6 P2 122.3(3) . .
C5 C7 C6 117.3(4) 2_444 .
C5 C7 C8 119.6(4) 2_444 .
C6 C7 C8 123.1(4) . .
N1 C9 C11 124.3(4) . .
N1 C10 C12 123.0(4) . .
C9 C11 C13 120.1(4) . .
C10 C12 C13 119.9(4) . .
C11 C13 C12 116.5(4) . .
C11 C13 C14 119.6(4) . .
C12 C13 C14 123.9(4) . .
C14 C14 C13 126.4(6) 2_656 .
N2 C15 C17 124.5(4) . .
N2 C16 C18 123.1(4) . .
C15 C17 C19 119.3(4) . .
C16 C18 C19 121.1(4) . .
C17 C19 C18 116.1(4) . .
C17 C19 C20 123.2(4) . .
C18 C19 C20 120.7(4) . .
C20 C20 C19 126.1(5) 2_544 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O6 2.048(3) .
Ni1 O3 2.072(3) .
Ni1 O1W 2.097(3) .
Ni1 N1 2.108(3) .
Ni1 O2W 2.109(3) .
Ni1 N2 2.118(3) .
O1 P1 1.563(3) .
O2 P1 1.513(3) .
O3 P1 1.504(3) .
O4 P2 1.513(3) .
O5 P2 1.580(3) .
O6 P2 1.497(3) .
N1 C9 1.326(5) .
N1 C10 1.347(5) .
N2 C15 1.336(5) .
N2 C16 1.339(5) .
P1 C2 1.806(4) .
P2 C6 1.809(4) .
C1 C3 1.388(5) 2_556
C1 C2 1.395(5) .
C2 C3 1.389(5) .
C3 C1 1.388(5) 2_556
C3 C4 1.521(6) .
C5 C6 1.380(5) .
C5 C7 1.389(5) 2_444
C6 C7 1.409(6) .
C7 C5 1.389(5) 2_444
C7 C8 1.508(6) .
C9 C11 1.376(6) .
C10 C12 1.384(6) .
C11 C13 1.375(6) .
C12 C13 1.392(6) .
C13 C14 1.467(6) .
C14 C14 1.305(8) 2_656
C15 C17 1.378(6) .
C16 C18 1.367(6) .
C17 C19 1.385(6) .
C18 C19 1.386(6) .
C19 C20 1.460(6) .
C20 C20 1.312(8) 2_544
