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_7718946
_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         'C6 F4 O12 Sb2, 2(H2 O), 4(H4 N)'
_chemical_formula_sum            'C6 H20 F4 N4 O14 Sb2'
_chemical_formula_weight         691.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-02-27
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-04-01 deposited with the CCDC.	2025-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.628(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.6392(5)
_cell_length_b                   9.8051(5)
_cell_length_c                   11.7908(6)
_cell_measurement_reflns_used    9398
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.506
_cell_measurement_theta_min      3.501
_cell_volume                     995.52(9)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'Bruker PHOTON-II area detector'
_diffrn_detector_area_resol_mean 7.4
_diffrn_detector_type            'CMOS-PHOTONII area detector'
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTON-II area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            29432
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.511
_diffrn_reflns_theta_min         2.705
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.825
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0993 before and 0.0615 after correction.
The Ratio of minimum to maximum transmission is 0.8962.
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    2.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2229
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0226
_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^)+(0.0282P)^2^+1.3996P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0623
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2050
_reflns_number_total             2229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01253h2.cif
_cod_data_source_block           86-b
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7718945--7718946.cif.
;
_cod_database_code               7718946
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.765
_shelx_estimated_absorpt_t_min   0.710
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
O8 \\sim O8A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
3. Others
 Sof(O8A)=Sof(H8AA)=Sof(H8AB)=1-FVAR(1)
 Sof(O8)=Sof(H8A)=Sof(H8B)=FVAR(1)
4.a Riding coordinates:
 N9(H9A), N9(H9B,H9C,H9D), N7(H7A), N7(H7B,H7C,H7D), O8(H8A,H8B), O8A(H8AA,H8AB)
;
_shelx_res_checksum              59154
_shelx_hkl_checksum              89164
_olex2_submission_special_instructions 'No special instructions were received'