{PMo6O24N4} subunit functionalized by organonitrogen through Mo‒N bonds: hydrothermal synthesis, structure, photocatalytic, and fluorescence sensing properties
Yu, Haiyan; Ying, Jun; Sun, Chenxi; Jin, Liang; Tian, Aixiang; Wang, Xiuli; New Journal of Chemistry 45 (2021) 7942–7945; doi:10.1039/D1NJ00887K

data_7060504
_publ_section_title
;
 {PMo6O24N4} subunit functionalized by organonitrogen through Mo--N bonds:
 hydrothermal synthesis, structure, photocatalytic, and fluorescence
 sensing properties
;
_journal_issue                   18
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7942
_journal_page_last               7945
_journal_paper_doi               10.1039/D1NJ00887K
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C24 H40 Cd3 Mo12 N12 O56 P2, H4 O2'
_chemical_formula_sum            'C24 H44 Cd3 Mo12 N12 O58 P2'
_chemical_formula_weight         2979.13
_chemical_name_systematic        'Compound 1'
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-11
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.10.31 svn.r3677 for OlexSys, GUI svn.r5972)
;
_audit_update_record
;
2020-11-12 deposited with the CCDC.	2021-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                81.484(3)
_cell_angle_beta                 75.196(3)
_cell_angle_gamma                77.313(3)
_cell_formula_units_Z            1
_cell_length_a                   10.2923(18)
_cell_length_b                   10.3806(18)
_cell_length_c                   17.587(3)
_cell_measurement_reflns_used    4216
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.25
_cell_volume                     1763.8(5)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.989
_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  0.0269
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12717
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.320
_diffrn_reflns_theta_min         1.203
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.106
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0583 before and 0.0354 after correction.
The Ratio of minimum to maximum transmission is 0.8098.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.805
_exptl_crystal_description       block
_exptl_crystal_F_000             1414
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         4.054
_refine_diff_density_min         -1.886
_refine_diff_density_rms         0.330
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         8690
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0543
_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^)+(0.0959P)^2^+4.3879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1642
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6398
_reflns_number_total             8690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj00887k2.cif
_cod_data_source_block           2
_cod_depositor_comments          'Adding full bibliography for 7060504.cif.'
_cod_database_code               7060504
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.6079
_shelx_estimated_absorpt_t_min   0.5568
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H1WA,H1WB} of O1W, All C(H,H) groups
 At 1.5 times of:
  {H3A,H3B} of O3, {H19A,H19B} of O19, {H1A,H1B} of O1, {H2A,H2B} of O2
2. Restrained distances
 Cd2-H1A \\sim Cd2-H1B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1W: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(O1W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(P1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 O1W
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5.a Riding coordinates:
 O1W(H1WA,H1WB)
5.b Free rotating group:
 O1(H1A,H1B), O3(H3A,H3B), O2(H2A,H2B)
5.c Rotating group:
 O19(H19A,H19B)
5.d Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C3(H3C,H3D)
5.e Aromatic/amide H refined with riding coordinates:
 C8(H8), C11(H11), C2(H2), C7(H7), C12(H12), C5(H5), C1(H1), C6(H6)
;
_shelx_res_checksum              20791
_olex2_submission_special_instructions 'No special instructions were received'