A new polar glass-ceramic built from monovalent perrhenate anions and large methyltriphenylphosphonium cations.
Pan, Xiong; Fang, Zi-Luo; Guo, Ming-Yu; Yang, Hao; Zhang, Wei-Xiong; Chemical communications (Cambridge, England) 62 (2026) 4302–4305; doi:10.1039/d5cc07096a

data_7135417
_publ_section_title
;
 A new polar glass-ceramic built from monovalent perrhenate anions and
 large methyltriphenylphosphonium cations.
;
_journal_issue                   14
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4302
_journal_page_last               4305
_journal_paper_doi               10.1039/d5cc07096a
_journal_volume                  62
_journal_year                    2026
_chemical_absolute_configuration ad
_chemical_formula_moiety         'O4 Re, C19 H18 P'
_chemical_formula_sum            'C19 H18 O4 P Re'
_chemical_formula_weight         527.50
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2025-10-02
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-12-11 deposited with the CCDC.	2026-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.0665(3)
_cell_length_b                   12.9576(3)
_cell_length_c                   19.5981(5)
_cell_measurement_reflns_used    10629
_cell_measurement_temperature    250.01(10)
_cell_measurement_theta_max      78.3040
_cell_measurement_theta_min      4.4620
_cell_volume                     3826.05(15)
_computing_cell_refinement       'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.144a 64-bit (release 23-01-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      250.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     43.00 102.00   0.50    0.20    --  115.25 -77.00  90.00  118
  2  \w     50.00  98.00   0.50    0.20    --  115.25 -77.00  60.00   96
  3  \w     50.00  93.00   0.50    0.20    --  115.25 -77.00   0.00   86
  4  \w     55.00  87.00   0.50    0.20    --  115.25 -77.00 150.00   64
  5  \w     67.00  93.00   0.50    0.20    --  115.25 -77.00 -30.00   52
  6  \w     50.00  77.00   0.50    0.20    --  115.25 -77.00-120.00   54
  7  \w     51.00  88.00   0.50    0.20    --  115.25 -77.00-150.00   74
  8  \w    -11.00  17.00   0.50    0.05    --   47.65 -19.00 -90.00   56
  9  \w     33.00 120.00   0.50    0.05    --   47.65  38.00-122.00  174
 10  \w     98.00 138.00   0.50    0.20    --  115.25  61.00 -30.00   80
 11  \w    113.00 175.00   0.50    0.20    --  115.25  83.00  38.00  124
 12  \w     75.00 111.00   0.50    0.05    --   47.65 137.00 -80.00   72
 13  \w    101.00 175.00   0.50    0.20    --  115.25  61.00-150.00  148
 14  \w     43.00  86.00   0.50    0.20    --  115.25 -95.00 -30.00   86
 15  \w     45.00 101.00   0.50    0.20    --  115.25-137.00-142.00  112
 16  \w     47.00 111.00   0.50    0.20    --  115.25-125.00-120.00  128
 17  \w    -67.00 -27.00   0.50    0.20    --  -97.00  61.00 150.00   80
 18  \w    -54.00 -24.00   0.50    0.20    --  -97.00  45.00 120.00   60
 19  \w    -54.00 -24.00   0.50    0.20    --  -97.00  45.00  30.00   60
 20  \w    -50.00 -25.00   0.50    0.20    --  -97.00  45.00 -30.00   50
 21  \w    -53.00 -25.00   0.50    0.20    --  -97.00  45.00 -60.00   56
 22  \w    -45.00  26.00   0.50    0.05    --  -47.65  38.00  30.00  142
 23  \w   -130.00 -89.00   0.50    0.20    --  -97.00 -38.00  83.00   82
 24  \w    -97.00 -71.00   0.50    0.05    --  -47.65-179.00 -60.00   52
 25  \w   -164.00-139.00   0.50    0.20    --  -97.00-137.00-142.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0433098000
_diffrn_orient_matrix_UB_12      -0.0462429000
_diffrn_orient_matrix_UB_13      0.0640052000
_diffrn_orient_matrix_UB_21      -0.1107575000
_diffrn_orient_matrix_UB_22      0.0167992000
_diffrn_orient_matrix_UB_23      -0.0255376000
_diffrn_orient_matrix_UB_31      0.0015290000
_diffrn_orient_matrix_UB_32      -0.0895880000
_diffrn_orient_matrix_UB_33      -0.0378302000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0949
_diffrn_reflns_av_unetI/netI     0.0897
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26419
_diffrn_reflns_point_group_measured_fraction_full 0.898
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.983
_diffrn_reflns_theta_min         3.411
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.385
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.144a (Rigaku Oxford Diffraction, 2024)
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    1.832
_exptl_crystal_description       block
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.049
_refine_diff_density_min         -1.611
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.20(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         7101
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0514
_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/[\s^2^(Fo^2^)+(0.0583P)^2^+4.2182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1385
_refine_ls_wR_factor_ref         0.1453
_reflns_Friedel_coverage         0.676
_reflns_Friedel_fraction_full    0.790
_reflns_Friedel_fraction_max     0.708
_reflns_number_gt                6011
_reflns_number_total             7101
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc07096a2.cif
_cod_data_source_block           exp_13444_auto
_cod_database_code               7135417
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         ReOCP
_chemical_oxdiff_usercomment     CHZnI
_shelx_estimated_absorpt_t_max   0.690
_shelx_estimated_absorpt_t_min   0.554
_diffrn_oxdiff_ac3_digest_hkl    0126de929aad8a99744bb28b9e437cd7889681
_diffrn_oxdiff_digest_hkl
;
43181349a99b04cbdd8a84401e6dc4d9ba9421
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.80(3)
 0.20(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O3) \\sim
Ueq, Uanis(O6) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C35) \\sim Ueq,
Uanis(C30) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C26(H26), C25(H25), C24(H24),
 C23(H23), C22(H22), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C32(H32),
 C31(H31), C30(H30), C29(H29), C28(H28), C18(H18), C17(H17), C16(H16), C15(H15),
  C14(H14), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38)
4.b Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C21(C26,C25,C24,C23,C22), C7(C8,C9,C10,C11,C12), C27(C32,
 C31,C30,C29,C28), C13(C18,C17,C16,C15,C14), C33(C34,C35,C36,C37,C38)
4.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              26819
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.495
_oxdiff_exptl_absorpt_empirical_full_min 0.277