#------------------------------------------------------------------------------
#$Date: 2025-11-29 19:42:44 +0100 (Sat 29 de Nov de 2025) $
#$Revision: 303666 $
#$URL: svn://www.crystallography.net/cod/cif/1/57/58/1575876.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_1575876
loop_
_publ_author_name
'Karak, Shayan'
'Khata, Soubhik'
'Ahmad, Shamim'
'Yadav, Abhishek Kumar'
'AlMasoud, Najla'
'Alomar, Taghrid S.'
'Dharavath, Srinivas'
'Reddy, C. Malla'
'Banerjee, Rahul'
_publ_section_title
;
 Tunable mechanics and energetics in structurally diverse TNPG-based metal
 organic networks.
;
_journal_issue                   45
_journal_name_full               'Chemical science'
_journal_page_first              21508
_journal_page_last               21517
_journal_paper_doi               10.1039/d5sc04870b
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C3 H1.5 N1.5 O4.5'
_chemical_formula_sum            'C3 H1.5 N1.5 O4.5'
_chemical_formula_weight         130.56
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc2lm2dq
_audit_creation_date             2024-11-10
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-11-10 deposited with the CCDC.	2025-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   13.0013(4)
_cell_length_b                   13.0013(4)
_cell_length_c                   9.3490(4)
_cell_measurement_reflns_used    839
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.701
_cell_measurement_theta_min      3.619
_cell_volume                     1368.58(8)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'Four-circle Kappa diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9474
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.701
_diffrn_reflns_theta_min         3.619
_exptl_absorpt_coefficient_mu    0.185
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_description       Needle
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.283
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0204P)²+1.6278P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0879
_reflns_Friedel_coverage         0.000
_reflns_number_gt                787
_reflns_number_total             839
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5sc04870b2.cif
_cod_data_source_block           rb_sk_tnpg_a
_cod_depositor_comments
'Adding full bibliography for 1575876--1575880.cif.'
_cod_original_cell_volume        1368.58(10)
_cod_original_formula_sum        'C3 H1.50 N1.50 O4.50'
_cod_database_code               1575876
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Sof: H001(0.5)
3.a Idealised tetrahedral OH refined as rotating group:
 O001(H001), O005(H005)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 32 electrons were 
found in a volume of 64Å³ in 1 void per unit cell. 
This is consistent with the presence of 
1[H2O] per Asymmetric Unit 
which account for 120 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, 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
O001 O 1.000000 0.87309(13) 0.750000 0.0196(4) Uani 1 2 d S T P . .
H001 H 0.938749 0.864000 0.708355 0.029 Uiso 0.5 1 calc R U P . .
O002 O 0.75677(11) 0.59831(11) 0.51325(13) 0.0207(3) Uani 1 1 d . . . . .
O003 O 0.82330(11) 0.77680(11) 0.58945(13) 0.0209(3) Uani 1 1 d . . . . .
O004 O 0.91536(12) 0.35894(11) 0.80522(13) 0.0234(3) Uani 1 1 d . . . . .
O005 O 0.82901(12) 0.46403(11) 0.61438(14) 0.0246(4) Uani 1 1 d . . . . .
H005 H 0.787046 0.479459 0.560034 0.037 Uiso 1 1 calc R U . . .
N006 N 0.82659(12) 0.68343(13) 0.58854(14) 0.0167(3) Uani 1 1 d . . . . .
N007 N 1.000000 0.44508(16) 0.750000 0.0171(5) Uani 1 2 d S T P . .
C009 C 1.000000 0.55766(18) 0.750000 0.0162(5) Uani 1 2 d S T P . .
C00A C 1.000000 0.77157(18) 0.750000 0.0158(5) Uani 1 2 d S T P . .
C00B C 0.90964(15) 0.56250(15) 0.67720(17) 0.0166(4) Uani 1 1 d . . . . .
C00C C 0.91188(15) 0.67242(15) 0.67440(17) 0.0163(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'
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'
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
H001 O001 H001 141.1 . 6_766 ?
C00A O001 H001 109.470(15) . 6_766 ?
C00A O001 H001 109.5 . . ?
C00B O005 H005 109.5 . . ?
O002 N006 C00C 119.10(14) . . ?
O003 N006 O002 120.71(14) . . ?
O003 N006 C00C 120.19(14) . . ?
O004 N007 O004 124.5(2) . 6_766 ?
O004 N007 C009 117.73(10) 6_766 . ?
O004 N007 C009 117.73(10) . . ?
C00B C009 N007 117.98(11) . . ?
C00B C009 N007 117.97(11) 6_766 . ?
C00B C009 C00B 124.0(2) 6_766 . ?
O001 C00A C00C 120.45(11) . . ?
O001 C00A C00C 120.45(11) . 6_766 ?
C00C C00A C00C 119.1(2) 6_766 . ?
O005 C00B C009 117.05(16) . . ?
O005 C00B C00C 125.24(15) . . ?
C009 C00B C00C 117.71(16) . . ?
C00A C00C N006 120.26(16) . . ?
C00A C00C C00B 120.66(16) . . ?
C00B C00C N006 119.02(15) . . ?
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
O001 H001 0.8400 . ?
O001 H001 0.8400 6_766 ?
O001 C00A 1.320(3) . ?
O002 N006 1.2408(19) . ?
O003 N006 1.2360(19) . ?
O004 N007 1.2244(16) . ?
O005 H005 0.8400 . ?
O005 C00B 1.319(2) . ?
N006 C00C 1.433(2) . ?
N007 C009 1.464(3) . ?
C009 C00B 1.386(2) . ?
C009 C00B 1.386(2) 6_766 ?
C00A C00C 1.413(2) 6_766 ?
C00A C00C 1.413(2) . ?
C00B C00C 1.415(2) . ?
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
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O001 C00A C00C N006 4.48(17) . . . . ?
O001 C00A C00C C00B -178.31(11) . . . . ?
O002 N006 C00C C00A 173.69(13) . . . . ?
O002 N006 C00C C00B -3.6(2) . . . . ?
O003 N006 C00C C00A -6.0(2) . . . . ?
O003 N006 C00C C00B 176.69(15) . . . . ?
O004 N007 C009 C00B -62.23(10) . . . . ?
O004 N007 C009 C00B -62.23(10) 6_766 . . 6_766 ?
O004 N007 C009 C00B 117.77(10) 6_766 . . . ?
O004 N007 C009 C00B 117.77(10) . . . 6_766 ?
O005 C00B C00C N006 -5.2(3) . . . . ?
O005 C00B C00C C00A 177.59(14) . . . . ?
N007 C009 C00B O005 0.82(16) . . . . ?
N007 C009 C00B C00C -178.36(11) . . . . ?
C009 C00B C00C N006 173.94(12) . . . . ?
C009 C00B C00C C00A -3.3(2) . . . . ?
C00B C009 C00B O005 -179.19(16) 6_766 . . . ?
C00B C009 C00B C00C 1.63(11) 6_766 . . . ?
C00C C00A C00C N006 -175.52(17) 6_766 . . . ?
C00C C00A C00C C00B 1.69(11) 6_766 . . . ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 7.1 2.7 ?
2 0.000 0.000 0.500 7.1 2.7 ?
3 0.333 0.667 0.141 15.8 8.3 '0.75 H2O'
4 0.333 0.667 0.641 15.8 8.4 '0.75 H2O'
5 0.667 0.333 0.359 15.8 8.3 '0.75 H2O'
6 0.667 0.333 0.859 15.8 8.3 '0.75 H2O'
