#------------------------------------------------------------------------------
#$Date: 2025-08-21 14:03:24 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301848 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/82/7028299.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_7028299
loop_
_publ_author_name
'Schilling, Lars-Hendrik'
'Stock, Norbert'
_publ_section_title
;
 High-throughput ultrasonic synthesis and in situ crystallisation
 investigation of metal phosphonocarboxylates.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              414
_journal_page_last               422
_journal_paper_doi               10.1039/c3dt52576g
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C16 H24 Ni O14 P2'
_chemical_formula_sum            'C16 H24 Ni O14 P2'
_chemical_formula_weight         561.00
_chemical_name_systematic
; 
 bis(μ₂-4-(Phosphatomethyl)benzoic acid)-tetraaqua-nickel
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                83.42(3)
_cell_angle_beta                 89.71(3)
_cell_angle_gamma                83.50(3)
_cell_formula_units_Z            1
_cell_length_a                   4.7713(10)
_cell_length_b                   6.8621(14)
_cell_length_c                   16.598(3)
_cell_measurement_temperature    293(2)
_cell_volume                     536.37(19)
_computing_cell_refinement       'X-Area (Stoe, 2008)'
_computing_data_collection       'X-Area (Stoe, 2008)'
_computing_data_reduction        'X-Area (Stoe, 2008)'
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008) 
;
_computing_publication_material  'XCIF in SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Stoe IPSD-2'
_diffrn_measurement_method       'omega scan'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2458
_diffrn_reflns_theta_full        27.94
_diffrn_reflns_theta_max         27.94
_diffrn_reflns_theta_min         2.47
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.127
_exptl_absorpt_correction_T_max  0.9005
_exptl_absorpt_correction_T_min  0.7625
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape and X-Red32 (Stoe, 2008)'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             290
_exptl_crystal_size_max          0.1682
_exptl_crystal_size_mid          0.1136
_exptl_crystal_size_min          0.0822
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.762
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2458
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.762
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0320
_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)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0427
_refine_ls_wR_factor_ref         0.0429
_reflns_number_gt                2083
_reflns_number_total             2458
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52576g.txt
_cod_data_source_block           c:\einkris\nil6_ipds2\absc\nil6a
_cod_original_cell_volume        536.36(19)
_cod_database_code               7028299
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 0.5000 0.5000 0.5000 0.01830(10) Uani 1 2 d S
P1 P 0.34444(9) 0.76653(6) 0.64732(3) 0.01885(11) Uani 1 1 d .
O1 O 0.2562(2) 0.63184(17) 0.58896(7) 0.0228(3) Uani 1 1 d .
O2 O 0.0850(3) 0.91035(18) 0.66907(8) 0.0299(3) Uani 1 1 d .
H1 H -0.0722 0.8957 0.6527 0.036 Uiso 1 1 d R
O3 O 0.5741(3) 0.88994(17) 0.61515(7) 0.0233(3) Uani 1 1 d .
O4 O -0.4062(4) 0.2295(2) 0.98818(9) 0.0463(4) Uani 1 1 d .
O5 O -0.2881(4) -0.0172(2) 0.91411(11) 0.0528(5) Uani 1 1 d .
H2 H -0.3975 -0.0757 0.9435 0.082(11) Uiso 1 1 d R
O6 O 0.3288(3) 0.23525(17) 0.53114(8) 0.0240(3) Uani 1 1 d .
H3 H 0.3440 0.1921 0.4871 0.029 Uiso 1 1 d R
H4 H 0.4042 0.1467 0.5640 0.029 Uiso 1 1 d R
O7 O 0.1832(3) 0.58852(18) 0.41627(8) 0.0261(3) Uani 1 1 d .
H5 H 0.0764 0.6784 0.4320 0.031 Uiso 1 1 d R
H6 H 0.0810 0.4996 0.4202 0.031 Uiso 1 1 d R
C1 C 0.4736(4) 0.6338(3) 0.74137(12) 0.0291(4) Uani 1 1 d .
H1B H 0.6409 0.5469 0.7304 0.035 Uiso 1 1 calc R
H1A H 0.5307 0.7279 0.7757 0.035 Uiso 1 1 calc R
C2 C 0.2690(4) 0.5113(3) 0.78825(11) 0.0271(4) Uani 1 1 d .
C3 C 0.2329(5) 0.3235(3) 0.76917(12) 0.0335(5) Uani 1 1 d .
H3A H 0.3289 0.2743 0.7256 0.040 Uiso 1 1 calc R
C4 C 0.0546(5) 0.2094(3) 0.81474(12) 0.0328(5) Uani 1 1 d .
H4A H 0.0334 0.0834 0.8020 0.039 Uiso 1 1 calc R
C5 C -0.0924(4) 0.2816(3) 0.87924(12) 0.0281(4) Uani 1 1 d .
C6 C -0.0632(4) 0.4714(3) 0.89705(12) 0.0301(4) Uani 1 1 d .
H6A H -0.1645 0.5221 0.9395 0.036 Uiso 1 1 calc R
C7 C 0.1161(4) 0.5851(3) 0.85183(11) 0.0288(4) Uani 1 1 d .
H7A H 0.1346 0.7119 0.8641 0.035 Uiso 1 1 calc R
C8 C -0.2737(4) 0.1584(3) 0.93086(12) 0.0307(4) Uani 1 1 d .
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'
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
O7 Ni1 O7 180.00(5) 2_666 .
O7 Ni1 O6 89.93(6) 2_666 .
O7 Ni1 O6 90.07(6) . .
O7 Ni1 O6 90.07(6) 2_666 2_666
O7 Ni1 O6 89.93(5) . 2_666
O6 Ni1 O6 180.0 . 2_666
O7 Ni1 O1 89.69(5) 2_666 .
O7 Ni1 O1 90.31(5) . .
O6 Ni1 O1 90.49(5) . .
O6 Ni1 O1 89.51(5) 2_666 .
O7 Ni1 O1 90.31(5) 2_666 2_666
O7 Ni1 O1 89.69(5) . 2_666
O6 Ni1 O1 89.51(5) . 2_666
O6 Ni1 O1 90.49(5) 2_666 2_666
O1 Ni1 O1 180.00(6) . 2_666
O1 P1 O3 113.84(7) . .
O1 P1 O2 109.92(8) . .
O3 P1 O2 107.94(7) . .
O1 P1 C1 112.27(8) . .
O3 P1 C1 106.45(8) . .
O2 P1 C1 106.03(9) . .
P1 O1 Ni1 128.17(7) . .
P1 O2 H1 119.3 . .
C8 O5 H2 112.7 . .
Ni1 O6 H3 98.5 . .
Ni1 O6 H4 122.7 . .
H3 O6 H4 105.4 . .
Ni1 O7 H5 109.6 . .
Ni1 O7 H6 105.6 . .
H5 O7 H6 100.7 . .
C2 C1 P1 115.89(14) . .
C2 C1 H1B 108.3 . .
P1 C1 H1B 108.3 . .
C2 C1 H1A 108.3 . .
P1 C1 H1A 108.3 . .
H1B C1 H1A 107.4 . .
C7 C2 C3 119.02(17) . .
C7 C2 C1 120.12(17) . .
C3 C2 C1 120.85(18) . .
C4 C3 C2 120.33(19) . .
C4 C3 H3A 119.8 . .
C2 C3 H3A 119.8 . .
C5 C4 C3 120.47(19) . .
C5 C4 H4A 119.8 . .
C3 C4 H4A 119.8 . .
C4 C5 C6 119.39(17) . .
C4 C5 C8 121.17(18) . .
C6 C5 C8 119.42(17) . .
C7 C6 C5 120.17(18) . .
C7 C6 H6A 119.9 . .
C5 C6 H6A 119.9 . .
C6 C7 C2 120.57(18) . .
C6 C7 H7A 119.7 . .
C2 C7 H7A 119.7 . .
O4 C8 O5 123.02(18) . .
O4 C8 C5 119.42(17) . .
O5 C8 C5 117.56(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O7 2.0507(14) 2_666
Ni1 O7 2.0507(14) .
Ni1 O6 2.0860(13) .
Ni1 O6 2.0860(13) 2_666
Ni1 O1 2.0983(13) .
Ni1 O1 2.0984(13) 2_666
P1 O1 1.5057(13) .
P1 O3 1.5179(13) .
P1 O2 1.5611(14) .
P1 C1 1.790(2) .
O2 H1 0.8200 .
O4 C8 1.254(2) .
O5 C8 1.277(2) .
O5 H2 0.8200 .
O6 H3 0.8200 .
O6 H4 0.8199 .
O7 H5 0.8200 .
O7 H6 0.8200 .
C1 C2 1.514(3) .
C1 H1B 0.9700 .
C1 H1A 0.9700 .
C2 C7 1.390(3) .
C2 C3 1.391(3) .
C3 C4 1.384(3) .
C3 H3A 0.9300 .
C4 C5 1.385(3) .
C4 H4A 0.9300 .
C5 C6 1.390(3) .
C5 C8 1.480(3) .
C6 C7 1.384(3) .
C6 H6A 0.9300 .
C7 H7A 0.9300 .
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
O3 P1 O1 Ni1 29.54(11) .
O2 P1 O1 Ni1 150.76(8) .
C1 P1 O1 Ni1 -91.48(11) .
O7 Ni1 O1 P1 47.81(9) 2_666
O7 Ni1 O1 P1 -132.19(9) .
O6 Ni1 O1 P1 137.74(10) .
O6 Ni1 O1 P1 -42.26(10) 2_666
O1 Ni1 O1 P1 -132(40) 2_666
O1 P1 C1 C2 -59.35(17) .
O3 P1 C1 C2 175.46(14) .
O2 P1 C1 C2 60.70(16) .
P1 C1 C2 C7 -98.3(2) .
P1 C1 C2 C3 82.3(2) .
C7 C2 C3 C4 -2.2(3) .
C1 C2 C3 C4 177.1(2) .
C2 C3 C4 C5 0.8(3) .
C3 C4 C5 C6 1.1(3) .
C3 C4 C5 C8 -177.2(2) .
C4 C5 C6 C7 -1.5(3) .
C8 C5 C6 C7 176.86(19) .
C5 C6 C7 C2 0.0(3) .
C3 C2 C7 C6 1.9(3) .
C1 C2 C7 C6 -177.50(17) .
C4 C5 C8 O4 -179.2(2) .
C6 C5 C8 O4 2.5(3) .
C4 C5 C8 O5 0.5(3) .
C6 C5 C8 O5 -177.83(19) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168348109
