Histidine-directed synthesis and optical properties of two indium phosphite–oxalates with three-dimensional structures
Wen, Xuemei; Li, Ying; Zhao, Yan; Li, Jing; Zeng, Hongmei; Zou, Guohong; Lin, Zhien; CrystEngComm 27 (2025) 903–907; doi:10.1039/D4CE01135J

data_7249803
_publ_section_title
;
 Histidine-directed synthesis and optical properties of two indium
 phosphite--oxalates with three-dimensional structures
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              903
_journal_page_last               907
_journal_paper_doi               10.1039/D4CE01135J
_journal_volume                  27
_journal_year                    2025
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C10 H17 In4 N3 O28 P6, C6 H11 N3 O2'
_chemical_formula_sum            'C16 H28 In4 N6 O30 P6'
_chemical_formula_weight         1429.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-11-08 deposited with the CCDC.	2025-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.2920(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.3970(2)
_cell_length_b                   23.4886(8)
_cell_length_c                   9.9675(3)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.32
_cell_volume                     1866.59(10)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      300.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0756
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            45576
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.152
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.815
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5654
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.543
_exptl_crystal_description       prism
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.871
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.30(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         8561
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0321
_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/[\s^2^(Fo^2^)+(0.0281P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0732
_reflns_Friedel_coverage         0.951
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                7524
_reflns_number_total             8561
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01135j2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7249802--7249803.cif.'
_cod_database_code               7249803
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.840
_shelx_estimated_absorpt_t_min   0.532
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.70(3)
 0.30(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H,H) groups,
  All P(H) groups
 At 1.5 times of:
  All O(H) groups
3.a Riding coordinates:
 P1(H1), P2(H2), P3(H3), P4(H4), P5(H5), P6(H6)
3.b Ternary CH refined with riding coordinates:
 C6(H6B), C12(H12)
3.c Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C13(H13A,H13B)
3.d Aromatic/amide H refined with riding coordinates:
 N2(H2A), N3(H3A), C9(H9), C10(H10), N5(H5A), N6(H6C), C15(H15), C16(H16)
3.e Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N4(H4A,H4B,H4C)
3.f Idealised tetrahedral OH refined as rotating group:
 O6(H6A), O30(H30)
;
_shelx_res_checksum              21409
_shelx_hkl_checksum              80132
_olex2_submission_special_instructions 'No special instructions were received'