Synergistic effect of 2[V2P2O14]∞ layers and hydrogen bonds inducing large birefringence in M(VO)2(PO4)2·4H2O (M = Ca, Sr, Ba) system
Wang, Xinmei; Qi, Lu; Wu, Lei; Zhang, Ruixin; Abudoureheman, Maierhaba; Lv, Jiarong; Wang, Peng; Dong, Xiaoyu; Jing, Qun; Chen, Zhaohui; CrystEngComm  (2022) –; doi:10.1039/D2CE00728B

data_7245326
_publ_section_title
;
 Synergistic effect of 2[V2P2O14]\\infty layers and hydrogen bonds
 inducing large birefringence in M(VO)2(PO4)2&#x00B7;4H2O (M = Ca, Sr, Ba)
 system
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00728B
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'Ca H8 O14 P2 V2'
_chemical_formula_sum            'Ca H8 O14 P2 V2'
_chemical_formula_weight         435.96
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-04
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_audit_update_record
;
2022-02-23 deposited with the CCDC.	2022-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                85.841(7)
_cell_angle_beta                 73.143(7)
_cell_angle_gamma                89.946(6)
_cell_formula_units_Z            1
_cell_length_a                   6.3369(5)
_cell_length_b                   6.3410(5)
_cell_length_c                   6.5675(6)
_cell_measurement_reflns_used    6504
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.9720
_cell_measurement_theta_min      3.1920
_cell_volume                     251.84(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.917
_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    -40.00  62.00   1.00    1.00    --  -11.59  57.00  30.00  102
  2  \w    -85.00  17.00   1.00    1.00    --  -11.59 -57.00-120.00  102
  3  \w    -20.00  29.00   1.00    1.00    --  -11.59 -99.00  30.00   49
  4  \w     34.00  99.00   1.00    1.00    --   11.74-178.00-120.00   65
  5  \w    -21.00  80.00   1.00    1.00    --   11.74  77.00  90.00  101
  6  \w     35.00 101.00   1.00    1.00    --   11.74 178.00   0.00   66
  7  \w     10.00  43.00   1.00    1.00    --   11.74 -77.00 -60.00   33
  8  \w     -3.00  72.00   1.00    1.00    --   11.74  37.00  60.00   75
  9  \w     17.00  52.00   1.00    1.00    --   11.74 -99.00 120.00   35
 10  \w     20.00  74.00   1.00    1.00    --   11.74  37.00-150.00   54
 11  \w    -35.00  -8.00   1.00    1.00    --   11.74 -77.00 -60.00   27
 12  \w    -66.00 -41.00   1.00    1.00    --  -11.59 122.00 136.46   25
 13  \w    -87.00 -38.00   1.00    1.00    --  -11.59 153.00-105.69   49
 14  \w   -100.00  77.00   1.00    1.00    --  -11.59   0.00-180.00  177
 15  \w   -100.00  77.00   1.00    1.00    --  -11.59   0.00-150.00  177
 16  \w   -100.00  77.00   1.00    1.00    --  -11.59   0.00-120.00  177
 17  \w   -100.00  77.00   1.00    1.00    --  -11.59   0.00 -90.00  177
 18  \w    -60.00  15.00   1.00    1.00    --   11.74 -57.00 -90.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0000370000
_diffrn_orient_matrix_UB_12      -0.0350138000
_diffrn_orient_matrix_UB_13      0.1050440000
_diffrn_orient_matrix_UB_21      -0.0089584000
_diffrn_orient_matrix_UB_22      0.1060536000
_diffrn_orient_matrix_UB_23      0.0287024000
_diffrn_orient_matrix_UB_31      -0.1166387000
_diffrn_orient_matrix_UB_32      -0.0105231000
_diffrn_orient_matrix_UB_33      0.0308228000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            10713
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.864
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.561
_diffrn_reflns_theta_min         3.222
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.768
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
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    2.875
_exptl_crystal_description       block
_exptl_crystal_F_000             216
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.434
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.181
_refine_ls_abs_structure_details
;
 Flack x determined using 1057 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.038(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2444
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0548P)^2^+0.9695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1040
_reflns_Friedel_coverage         0.884
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.811
_reflns_number_gt                2379
_reflns_number_total             2444
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00728b2.cif
_cod_data_source_block           1
_cod_database_code               7245326
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.769
_shelx_estimated_absorpt_t_min   0.682
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Riding coordinates:
 O9(H9B,H9A), O12(H12B,H12A), O13(H13A,H13B), O14(H14A,H14B)
;
_shelx_res_checksum              69911
_shelx_hkl_checksum              38838
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.582
_oxdiff_exptl_absorpt_empirical_full_min 0.697