Unprecedented boat-shaped [Mo2O5(IO3)4]2- polyanions induced strong second harmonic generation response
Zeng, Wei; Dong, Xuehua; Tian, Yao; Huang, Ling; Zeng, Hongmei; Lin, Zhien; Zou, Guohong; Chemical Communications  (2022) –; doi:10.1039/D2CC00134A

data_7129718
_publ_section_title
;
 Unprecedented boat-shaped [Mo2O5(IO3)4]2- polyanions induced strong
 second harmonic generation response
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC00134A
_journal_year                    2022
_chemical_formula_moiety         'H2 I4 Mo2 O18, H2 O, 2(C H6 N3)'
_chemical_formula_sum            'C2 H15 I4 Mo2 N6 O19'
_chemical_formula_weight         1126.68
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-09-23 deposited with the CCDC.	2022-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.8979(5)
_cell_length_b                   13.1994(3)
_cell_length_c                   7.8514(2)
_cell_measurement_reflns_used    17313
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.8060
_cell_measurement_theta_min      2.2730
_cell_volume                     2476.63(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.886
_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     -4.00  74.00   0.50    0.33    --    4.56  77.00 120.00  156
  2  \w     -6.00  77.00   0.50    0.33    --    4.56  37.00  60.00  166
  3  \w    -21.00  38.00   0.50    0.33    --    4.56 -99.00 -60.00  118
  4  \w    -21.00  34.00   0.50    0.33    --    4.56 -99.00 -30.00  110
  5  \w      2.00  28.00   0.50    0.33    --   -5.65 -99.00  60.00   52
  6  \w    -78.00 -35.00   0.50    0.33    --   -5.65 -57.00-150.00   86
  7  \w     -1.00  18.50   0.50    0.33    --   -5.65 -99.00 150.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0141527000
_diffrn_orient_matrix_UB_12      -0.0115250000
_diffrn_orient_matrix_UB_13      0.0467288000
_diffrn_orient_matrix_UB_21      0.0258114000
_diffrn_orient_matrix_UB_22      -0.0067189000
_diffrn_orient_matrix_UB_23      -0.0262039000
_diffrn_orient_matrix_UB_31      0.0037754000
_diffrn_orient_matrix_UB_32      0.0893735000
_diffrn_orient_matrix_UB_33      0.0040639000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            31269
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.794
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.926
_diffrn_reflns_theta_min         2.299
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.087
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.59a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    3.022
_exptl_crystal_description       'New Gemini, Dual, Cu at zero, EosS2'
_exptl_crystal_F_000             2068
_refine_diff_density_max         2.885
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.220
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         6226
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0522P)^2^+4.9427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0911
_reflns_Friedel_coverage         0.680
_reflns_Friedel_fraction_full    0.936
_reflns_Friedel_fraction_max     0.688
_reflns_number_gt                5540
_reflns_number_total             6226
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00134a2.cif
_cod_data_source_block           5
_cod_database_code               7129718
_shelx_shelxl_version_number     2018/3
_diffrn_oxdiff_digest_frames
;
017013c837595d93800f5330efc52051fd00042c312
;
_diffrn_oxdiff_digest_hkl
;
015fc6b961d6216ca48ea53c07a7ffe2db178f
;
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.94(3)
 0.06(3)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups, All O(H,H) groups
3.a Riding coordinates:
 O18(H18A,H18B), O19(H19), O19(H1)
3.b X=CH2 refined with riding coordinates:
 N3(H3A,H3B), N4(H4A,H4B), N2(H2A,H2B), N6(H6A,H6B), N5(H5A,H5B), N1(H1A,H1B)
;
_shelx_res_checksum              32116
_shelx_hkl_checksum              81411
_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 1.734
_oxdiff_exptl_absorpt_empirical_full_min 0.681