Hydrothermal synthesis and structure of organically templated layered neptunyl(vi) phosphate (NpO2)3(PO4)2(Terpy)
Zhang, Lei; Wang, Yu; Xu, Mengyu; Kokot, Alex M.; Qiu, Jie; Burns, Peter C.; CrystEngComm 26 (2024) 5991–5995; doi:10.1039/D4CE00121D

data_7249449
_publ_section_title
;
 Hydrothermal synthesis and structure of organically templated layered
 neptunyl(vi) phosphate (NpO2)3(PO4)2(Terpy)
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              5991
_journal_page_last               5995
_journal_paper_doi               10.1039/D4CE00121D
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C15 H11 N3 Np3 O14 P2'
_chemical_formula_sum            'C15 H11 N3 Np3 O14 P2'
_chemical_formula_weight         1230.21
_chemical_name_common            (NpO2)3(PO4)2(Terpy)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-10-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-10-08 deposited with the CCDC.	2024-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9944(8)
_cell_length_b                   12.1989(7)
_cell_length_c                   13.1277(8)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    298
_cell_measurement_theta_max      28.77
_cell_measurement_theta_min      2.21
_cell_volume                     2241.1(2)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2015)'
_computing_data_collection       'Bruker APEX-3 (Bruker, 2015)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'combination of \w and \f-scans '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25503
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.737
_diffrn_reflns_theta_min         1.669
_exptl_absorpt_coefficient_mu    14.031
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Krause 2015)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.646
_exptl_crystal_description       plate
_exptl_crystal_F_000             2172
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.002
_refine_diff_density_max         2.055
_refine_diff_density_min         -1.314
_refine_diff_density_rms         0.182
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.635(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         5463
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0180
_refine_ls_R_factor_gt           0.0176
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+2.2376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0452
_refine_ls_wR_factor_ref         0.0455
_reflns_Friedel_coverage         0.872
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.916
_reflns_number_gt                5368
_reflns_number_total             5463
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00121d2.cif
_cod_data_source_block           lei
_cod_depositor_comments          'Adding full bibliography for 7249449.cif.'
_cod_database_code               7249449
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.767
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.365(18)
 0.635(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12),
 C13(H13), C14(H14)
3.b Fitted hexagon refined as free rotating group:
 N1(C1,C2,C3,C4,C5), N2(C6,C7,C8,C9,C10), N3(C11,C12,C13,C14,C15)
;
_shelx_res_checksum              6539
_shelx_hkl_checksum              42944
_olex2_submission_special_instructions 'No special instructions were received'