Chiral polyoxomolybdate-based hybrid compounds obtained by spontaneous resolution: syntheses, structures and non-linear optical properties
Hou, Yujiao; An, Haiyan; Xu, Tieqi; Zhao, Sangen; Luo, Junhua; New J. Chem. 40 (2016) 10316–; doi:10.1039/C6NJ02709A

data_7055842
_publ_section_title
;
 Chiral polyoxomolybdate-based hybrid compounds obtained by spontaneous
 resolution: syntheses, structures and non-linear optical properties
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              10316
_journal_paper_doi               10.1039/C6NJ02709A
_journal_volume                  40
_journal_year                    2016
_chemical_formula_sum            'C6 H30 Mo6 N3 Na2 O34.5 Se'
_chemical_formula_weight         1396.91
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2016-02-02 deposited with the CCDC.
2016-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.215(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.6276(5)
_cell_length_b                   13.9826(7)
_cell_length_c                   11.8503(7)
_cell_measurement_reflns_used    8302
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.996
_cell_measurement_theta_min      1.870
_cell_volume                     1770.67(16)
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 0.01
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8302
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.870
_exptl_absorpt_coefficient_mu    3.232
_exptl_absorpt_correction_T_max  0.531
_exptl_absorpt_correction_T_min  0.490
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1342
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.241
_refine_diff_density_min         -0.923
_refine_diff_density_rms         0.157
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.052(15)
_refine_ls_extinction_coef       0.0036(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         4969
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0275
_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^)+(0.0263P)^2^+1.5534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0722
_reflns_Friedel_coverage         0.914
_reflns_Friedel_fraction_full    0.972
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4893
_reflns_number_total             4969
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj02709a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7055840--7055842.cif.'
_cod_original_formula_sum        'C6 H30 Mo6 N3 Na2 O34.50 Se'
_cod_database_code               7055842
_shelxl_version_number           2014-3
_shelx_res_checksum              80607