A highly birefringent metal-free crystal assembled by cooperative non-covalent interactions.
Li, Yanqiang; Zhou, Yang; Ahmed, Belal; Xu, Qianting; Huang, Weiqi; Song, Yipeng; Song, Xianyu; Chen, Bin; Luo, Junhua; Zhao, Sangen; Materials horizons 11 (2024) 4393–4399; doi:10.1039/d4mh00422a

data_1571963
_publ_section_title
;
 A highly birefringent metal-free crystal assembled by cooperative
 non-covalent interactions.
;
_journal_issue                   18
_journal_name_full               'Materials horizons'
_journal_page_first              4393
_journal_page_last               4399
_journal_paper_doi               10.1039/d4mh00422a
_journal_volume                  11
_journal_year                    2024
_chemical_formula_moiety         'C6 H2 N7 O3, 2(H2 O), H4 N'
_chemical_formula_sum            'C6 H10 N8 O5'
_chemical_formula_weight         274.197
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_audit_creation_date             2024-04-25
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2024.04.08 svn.rfee37e2d for OlexSys, GUI svn.r6697)
;
_audit_update_record
;
2024-06-13 deposited with the CCDC.	2024-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.597(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.2242(2)
_cell_length_b                   34.8178(7)
_cell_length_c                   6.4291(1)
_cell_measurement_reflns_used    4633
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      72.3100
_cell_measurement_theta_min      4.9470
_cell_volume                     2062.69(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      200.15
_diffrn_measured_fraction_theta_full 0.9984
_diffrn_measured_fraction_theta_max 0.9764
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.9984
_diffrn_reflns_Laue_measured_fraction_max 0.9764
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            9189
_diffrn_reflns_point_group_measured_fraction_full 0.9984
_diffrn_reflns_point_group_measured_fraction_max 0.9764
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         72.42
_diffrn_reflns_theta_min         4.80
_exptl_absorpt_coefficient_mu    1.338
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.116a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_description       slice
_exptl_crystal_F_000             1141.105
_exptl_crystal_size_max          0.119
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.022
_refine_diff_density_max         0.2423
_refine_diff_density_min         -0.1862
_refine_diff_density_rms         0.0472
_refine_ls_d_res_high            0.8087
_refine_ls_d_res_low             9.2147
_refine_ls_extinction_coef       0.00032(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0939
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     524
_refine_ls_number_reflns         3980
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.0935
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0241
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0290P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0669
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              42
_reflns_limit_k_min              0
_reflns_limit_l_max              7
_reflns_limit_l_min              0
_reflns_number_gt                3312
_reflns_number_total             3980
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4mh00422a2.cif
_cod_data_source_block           compound
_cod_depositor_comments
;
          Adding full bibliography for 1571963.cif.

2025-06-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C12 H20 N16 O10'
_cod_original_formula_weight         548.395
_cod_original_formula_moiety         '2(C6 H2 N7 O3), 4(H2 O), 2(H4 N)'
_cod_original_formula_units_Z            4
_cod_database_code               1571963
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Rigid body (RIGU) restrains
 H15a, N15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
;
_olex2_refine_details
;
Refinement using NoSpherA2, an implementation of
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021
NoSpherA2 implementation of HAR makes use of
tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
 - for a fragment of the crystal.
This fragment can be embedded in an electrostatic crystal field by employing cluster charges
or modelled using implicit solvation models, depending on the software used.
The following options were used:
   SOFTWARE:       ORCA 5.0
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Normal
   METHOD:         R2SCAN
   BASIS SET:      cc-pVTZ
   CHARGE:         0
   MULTIPLICITY:   1
   DATE:           2024-04-25_10-07-57
;
_olex2_submission_special_instructions 'No special instructions were received'