#------------------------------------------------------------------------------
#$Date: 2026-03-04 12:23:17 +0100 (Wed 04 de Mar de 2026) $
#$Revision: 304757 $
#$URL: svn://www.crystallography.net/cod/cif/7/72/04/7720488.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_7720488
loop_
_publ_author_name
'Pattnaik, Archana Kumari'
'Behera, Gobinda Chandra'
_publ_section_title
;
 From discrete to polymeric assemblies: exploring supramolecular
 structural diversity in transition metal phosphinates with N-donor
 ligands.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              694
_journal_page_last               709
_journal_paper_doi               10.1039/d5dt01622c
_journal_volume                  55
_journal_year                    2026
_chemical_formula_sum            'C34 H32 N2 Ni O6 P2'
_chemical_formula_weight         685.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-09-10 deposited with the CCDC.	2025-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.771(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.447(5)
_cell_length_b                   11.211(2)
_cell_length_c                   11.2987(16)
_cell_measurement_reflns_used    7964
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.72
_cell_measurement_theta_min      2.70
_cell_volume                     3346.1(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0841
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            27581
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.403
_diffrn_reflns_theta_min         2.649
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            palegreen
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       rod
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         4174
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0390
_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)+(0.0393P)²+4.1146P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1091
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3275
_reflns_number_total             4174
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5dt01622c2.cif
_cod_data_source_block           1_a
_cod_original_cell_volume        3346.0(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7720488
_shelx_shelxl_version_number     2018/3
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.500000 0.86685(3) 0.250000 0.02395(11) Uani 1 2 d S T P . .
P1 P 0.39418(2) 0.88627(5) 0.38231(5) 0.03123(14) Uani 1 1 d . . . . .
O1 O 0.42203(6) 0.94862(15) 0.48300(15) 0.0435(4) Uani 1 1 d . . . . .
N1 N 0.500000 0.68091(19) 0.250000 0.0286(5) Uani 1 2 d S T P . .
C1 C 0.33979(9) 0.9741(2) 0.3344(2) 0.0444(6) Uani 1 1 d . . . . .
O2 O 0.42353(6) 0.85809(12) 0.27547(14) 0.0321(3) Uani 1 1 d . . . . .
N2 N 0.500000 0.05372(19) 0.250000 0.0277(5) Uani 1 2 d S T P . .
C2 C 0.32775(15) 1.0771(3) 0.3929(4) 0.0804(11) Uani 1 1 d . . . . .
H2 H 0.347080 1.102063 0.459332 0.096 Uiso 1 1 calc R U . . .
C3 C 0.2857(2) 1.1440(4) 0.3506(5) 0.1082(17) Uani 1 1 d . . . . .
H3 H 0.277311 1.213676 0.389746 0.130 Uiso 1 1 calc R U . . .
O3 O 0.51832(7) 0.86702(13) 0.43442(14) 0.0325(3) Uani 1 1 d . . . . .
H3B H 0.4925(12) 0.885(2) 0.470(3) 0.049 Uiso 1 1 d . U . . .
H3A H 0.5396(12) 0.908(3) 0.459(3) 0.049 Uiso 1 1 d . U . . .
C4 C 0.25734(16) 1.1091(5) 0.2543(5) 0.1054(19) Uani 1 1 d . . . . .
H4 H 0.229640 1.154537 0.227858 0.126 Uiso 1 1 calc R U . . .
C5 C 0.26904(13) 1.0088(4) 0.1967(4) 0.0957(14) Uani 1 1 d . . . . .
H5 H 0.249463 0.984917 0.130339 0.115 Uiso 1 1 calc R U . . .
C6 C 0.30999(11) 0.9413(3) 0.2358(3) 0.0678(9) Uani 1 1 d . . . . .
H6 H 0.317791 0.872133 0.195095 0.081 Uiso 1 1 calc R U . . .
C7 C 0.36884(9) 0.7481(2) 0.4370(2) 0.0377(5) Uani 1 1 d . . . . .
C8 C 0.33896(12) 0.7471(3) 0.5334(3) 0.0626(8) Uani 1 1 d . . . . .
H8 H 0.330003 0.818857 0.568112 0.075 Uiso 1 1 calc R U . . .
C9 C 0.32212(16) 0.6407(4) 0.5793(3) 0.0810(12) Uani 1 1 d . . . . .
H9 H 0.301551 0.641467 0.643767 0.097 Uiso 1 1 calc R U . . .
C10 C 0.33536(14) 0.5356(3) 0.5310(3) 0.0757(11) Uani 1 1 d . . . . .
H10 H 0.324303 0.464292 0.563008 0.091 Uiso 1 1 calc R U . . .
C11 C 0.36474(13) 0.5341(3) 0.4361(4) 0.0711(10) Uani 1 1 d . . . . .
H11 H 0.373787 0.461669 0.403087 0.085 Uiso 1 1 calc R U . . .
C12 C 0.38144(11) 0.6400(2) 0.3877(3) 0.0527(7) Uani 1 1 d . . . . .
H12 H 0.401179 0.638113 0.321780 0.063 Uiso 1 1 calc R U . . .
C13 C 0.47582(10) 0.61951(17) 0.1634(2) 0.0365(5) Uani 1 1 d . . . . .
H13 H 0.458935 0.661463 0.102438 0.044 Uiso 1 1 calc R U . . .
C14 C 0.47478(10) 0.49655(18) 0.1602(2) 0.0390(5) Uani 1 1 d . . . . .
H14 H 0.457345 0.456964 0.098503 0.047 Uiso 1 1 calc R U . . .
C15 C 0.500000 0.4325(2) 0.250000 0.0307(6) Uani 1 2 d S T P . .
C16 C 0.500000 0.3013(2) 0.250000 0.0311(6) Uani 1 2 d S T P . .
C17 C 0.45598(9) 0.23755(17) 0.2254(2) 0.0349(5) Uani 1 1 d . . . . .
H17 H 0.425707 0.277366 0.207711 0.042 Uiso 1 1 calc R U . . .
C18 C 0.45723(8) 0.11498(17) 0.2274(2) 0.0318(5) Uani 1 1 d . . . . .
H18 H 0.427239 0.073131 0.212467 0.038 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'
N N 0.0061 0.0033 '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'
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'
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
_geom_angle_publ_flag
O2 Ni1 O2 174.53(8) . 2_655 ?
O2 Ni1 N1 87.27(4) . . ?
O2 Ni1 N1 87.27(4) 2_655 . ?
O2 Ni1 N2 92.73(4) . 1_565 ?
O2 Ni1 N2 92.73(4) 2_655 1_565 ?
N1 Ni1 N2 180.0 . 1_565 ?
O2 Ni1 O3 92.42(7) . . ?
O2 Ni1 O3 87.59(7) 2_655 . ?
N1 Ni1 O3 90.05(4) . . ?
N2 Ni1 O3 89.95(4) 1_565 . ?
O2 Ni1 O3 87.59(7) . 2_655 ?
O2 Ni1 O3 92.42(7) 2_655 2_655 ?
N1 Ni1 O3 90.05(4) . 2_655 ?
N2 Ni1 O3 89.95(4) 1_565 2_655 ?
O3 Ni1 O3 179.89(8) . 2_655 ?
O1 P1 O2 117.06(9) . . ?
O1 P1 C1 109.18(12) . . ?
O2 P1 C1 108.03(11) . . ?
O1 P1 C7 108.48(11) . . ?
O2 P1 C7 108.01(10) . . ?
C1 P1 C7 105.47(11) . . ?
C13 N1 C13 117.9(2) 2_655 . ?
C13 N1 Ni1 121.06(12) 2_655 . ?
C13 N1 Ni1 121.06(12) . . ?
C2 C1 C6 118.3(3) . . ?
C2 C1 P1 120.9(3) . . ?
C6 C1 P1 120.7(2) . . ?
P1 O2 Ni1 130.72(9) . . ?
C18 N2 C18 118.2(2) . 2_655 ?
C18 N2 Ni1 120.90(11) . 1_545 ?
C18 N2 Ni1 120.90(11) 2_655 1_545 ?
C1 C2 C3 118.8(4) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 H2 120.6 . . ?
C4 C3 C2 121.3(4) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
Ni1 O3 H3B 108(2) . . ?
Ni1 O3 H3A 119(2) . . ?
H3B O3 H3A 107(3) . . ?
C5 C4 C3 120.1(4) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.1(5) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C1 121.4(4) . . ?
C5 C6 H6 119.3 . . ?
C1 C6 H6 119.3 . . ?
C8 C7 C12 118.1(2) . . ?
C8 C7 P1 120.9(2) . . ?
C12 C7 P1 120.9(2) . . ?
C7 C8 C9 120.7(3) . . ?
C7 C8 H8 119.7 . . ?
C9 C8 H8 119.7 . . ?
C10 C9 C8 120.4(3) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C9 C10 C11 120.0(3) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C10 C11 C12 120.5(3) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C7 C12 C11 120.2(3) . . ?
C7 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
N1 C13 C14 122.9(2) . . ?
N1 C13 H13 118.6 . . ?
C14 C13 H13 118.6 . . ?
C13 C14 C15 119.4(2) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
C14 C15 C14 117.6(3) . 2_655 ?
C14 C15 C16 121.18(13) . . ?
C14 C15 C16 121.18(13) 2_655 . ?
C17 C16 C17 117.8(2) . 2_655 ?
C17 C16 C15 121.12(12) . . ?
C17 C16 C15 121.12(12) 2_655 . ?
C18 C17 C16 119.6(2) . . ?
C18 C17 H17 120.2 . . ?
C16 C17 H17 120.2 . . ?
N2 C18 C17 122.4(2) . . ?
N2 C18 H18 118.8 . . ?
C17 C18 H18 118.8 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O2 2.0589(15) . ?
Ni1 O2 2.0590(15) 2_655 ?
Ni1 N1 2.084(2) . ?
Ni1 N2 2.095(2) 1_565 ?
Ni1 O3 2.1164(16) . ?
Ni1 O3 2.1164(16) 2_655 ?
P1 O1 1.4982(17) . ?
P1 O2 1.5000(17) . ?
P1 C1 1.805(3) . ?
P1 C7 1.809(2) . ?
N1 C13 1.334(2) 2_655 ?
N1 C13 1.334(2) . ?
C1 C2 1.376(4) . ?
C1 C6 1.383(4) . ?
N2 C18 1.337(2) . ?
N2 C18 1.337(2) 2_655 ?
C2 C3 1.405(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.350(7) . ?
C3 H3 0.9300 . ?
O3 H3B 0.83(3) . ?
O3 H3A 0.77(3) . ?
C4 C5 1.343(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.376(5) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.377(4) . ?
C7 C12 1.381(4) . ?
C8 C9 1.383(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.352(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.355(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.387(4) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.379(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.387(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.471(4) . ?
C16 C17 1.383(3) . ?
C16 C17 1.383(3) 2_655 ?
C17 C18 1.375(3) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
