Novel antimony phosphates with enlarged birefringence induced by lone pair cations.
Hu, Mei; Wang, Jialong; Tuerhong, Nuerbiye; Zhang, Zhiyuan; Jing, Qun; Chen, Zhaohui; Yang, Yonglei; Lee, Ming-Hsien; Dalton transactions (Cambridge, England : 2003) 53 (2024) 3377–3385; doi:10.1039/d3dt03833e

data_7715035
_publ_section_title
;
 Novel antimony phosphates with enlarged birefringence induced by lone
 pair cations.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3377
_journal_page_last               3385
_journal_paper_doi               10.1039/d3dt03833e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'H4 O19 P4 Sb4, 2(H4 N)'
_chemical_formula_sum            'H12 N2 O19 P4 Sb4'
_chemical_formula_weight         955.00
_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   difmap
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-02-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-09-20 deposited with the CCDC.	2024-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                85.297(4)
_cell_angle_beta                 81.574(4)
_cell_angle_gamma                70.609(3)
_cell_formula_units_Z            2
_cell_length_a                   7.2569(5)
_cell_length_b                   7.3904(5)
_cell_length_c                   18.9055(14)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    298.00
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.09
_cell_volume                     945.49(12)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.0610
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            49817
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_min         2.179
_exptl_absorpt_coefficient_mu    6.089
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1422 before and 0.0679 after correction.
The Ratio of minimum to maximum transmission is 0.8754.
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    3.354
_exptl_crystal_description       block
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.083
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.237
_refine_diff_density_min         -0.950
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4314
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0080P)^2^+3.2026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0450
_refine_ls_wR_factor_ref         0.0508
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3734
_reflns_number_total             4314
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03833e2.cif
_cod_data_source_block           sbponh
_cod_depositor_comments
'Adding full bibliography for 7715034--7715035.cif.'
_cod_database_code               7715035
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.751
_shelx_estimated_absorpt_t_min   0.632
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All N(H,H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O18) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Riding coordinates:
 O15(H15), O18(H18A,H18B), O19(H19), N1(H1A,H1B,H1C,H1D), N2(H2A,H2B,H2C,H2D)
;
_olex2_submission_special_instructions 'No special instructions were received'