Structural chemistry of antimony(III) oxalates with lone pairs: polyhedral distortion [SbO<sub>4</sub>F<sub>2</sub>], π-conjugation [C<sub>2</sub>O<sub>4</sub>], and birefringence tuning.
Zhang, Yunxiao; Xu, Guangsheng; Li, Ke; Jia, Wei; Dong, Xiaoyu; Dalton transactions (Cambridge, England : 2003) 54 (2025) 11078–11083; doi:10.1039/d5dt01253h

data_7718945
_publ_section_title
;
 Structural chemistry of antimony(III) oxalates with lone pairs:
 polyhedral distortion [SbO<sub>4</sub>F<sub>2</sub>], &#x3c0;-conjugation
 [C<sub>2</sub>O<sub>4</sub>], and birefringence tuning.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11078
_journal_page_last               11083
_journal_paper_doi               10.1039/d5dt01253h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C4 F2 O8 Sb, 2(H2 O), 3(C H6 N3)'
_chemical_formula_sum            'C7 H22 F2 N9 O10 Sb'
_chemical_formula_weight         552.08
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-11
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-04-01 deposited with the CCDC.	2025-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                69.660(3)
_cell_angle_beta                 76.132(3)
_cell_angle_gamma                69.725(3)
_cell_formula_units_Z            2
_cell_length_a                   8.3223(7)
_cell_length_b                   11.0455(9)
_cell_length_c                   12.2379(8)
_cell_measurement_reflns_used    7013
_cell_measurement_temperature    290.00
_cell_measurement_theta_max      25.24
_cell_measurement_theta_min      2.63
_cell_volume                     980.32(13)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      290.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_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  0.0970
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24593
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.587
_diffrn_reflns_theta_min         2.054
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.493
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6678
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1358 before and 0.0827 after correction.
The Ratio of minimum to maximum transmission is 0.8957.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.870
_exptl_crystal_description       block
_exptl_crystal_F_000             552
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.875
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       0.0026(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         4497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0386
_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^)+1.2806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0809
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3741
_reflns_number_total             4497
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01253h2.cif
_cod_data_source_block           3-1
_cod_depositor_comments
'Adding full bibliography for 7718945--7718946.cif.'
_cod_database_code               7718945
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1.a Free rotating group:
 O10(H10A,H10B), O9(H9C,H9D)
1.b X=CH2 refined with riding coordinates:
 N4(H4A,H4B), N8(H8A,H8B), N5(H5A,H5B), N1(H1A,H1B), N3(H3A,H3B), N2(H2A,H2B),
 N6(H6A,H6B), N9(H9A,H9B), N7(H7A,H7B)
;
_shelx_res_checksum              58675
_shelx_hkl_checksum              58378
_olex2_submission_special_instructions 'No special instructions were received'