Tris functionalized Cu-centered cyclohexamolybdate molecular armor as bimetallic catalyst for rapid p-nitrophenol hydrogenation
Fang, Qihua; fu, junhong; Wang, Fei; Qin, Zhaoxian; Ma, Weiguang; Zhang, Jiangwei; Li, Gao; New Journal of Chemistry 43 (2019) 28–36; doi:10.1039/C8NJ04265A

data_7057972
_publ_section_title
;
 Tris functionalized Cu-centered cyclohexamolybdate molecular armor as
 bimetallic catalyst for rapid p-nitrophenol hydrogenation
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              28
_journal_page_last               36
_journal_paper_doi               10.1039/C8NJ04265A
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety
'C8 H16 Cu Mo6 N2 O24, 0.13(H8 N4), 7(H2 O), 2(H4 N)'
_chemical_formula_sum            'C8 H39 Cu Mo6 N4.5 O31'
_chemical_formula_weight         1333.61
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n'
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-11-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-12 deposited with the CCDC.
2018-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6347(4)
_cell_length_b                   16.6347(4)
_cell_length_c                   12.9722(5)
_cell_measurement_reflns_used    3715
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.498
_cell_measurement_theta_min      2.909
_cell_volume                     3589.58(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,Version 1.171.39.46 
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,Version 1.171.39.46 
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,Version 1.171.39.46 
;
_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_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10087
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.498
_diffrn_reflns_theta_min         2.909
_exptl_absorpt_coefficient_mu    2.718
_exptl_absorpt_correction_T_max  0.762
_exptl_absorpt_correction_T_min  0.526
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,Version 1.171.39.46 
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2590
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3715
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0369P)^2^+5.2787P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0823
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3146
_reflns_number_total             3715
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj04265a2.cif
_cod_data_source_block           exp_680
_cod_original_cell_volume        3589.6(2)
_cod_original_formula_sum        'C8 H39 Cu Mo6 N4.50 O31'
_cod_database_code               7057972
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, {H1A,H1B} of N1
 At 1.5 times of:
  All O(H,H) groups, {H3C,H3D} of N3, {H2C,H2D} of N2
2. Restrained distances
 N1-H1A = N1-H1B
 0.8 with sigma of 0.02
 H2E-H2F = H2C-H2F
 1.6 with sigma of 0.02
 N2-H2F
 0.8 with sigma of 0.02
 H2C-H2D \\sim H2C-H2E \\sim H2D-H2E
 with sigma of 0.02
3. Others
 Fixed Sof: H3C(0.25) H3D(0.25) H14A(0.5) H14B(0.5)
4.a Free rotating group:
 N3(H3C,H3D), O13(H13A,H13B), N2(H2C,H2D), O14(H14A,H14B), O16(H16A,H16B),
 O15(H15A,H15B)
4.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B), C4(H4A,H4B)
;
_shelx_res_checksum              29875
_shelx_hkl_checksum              1918
_olex2_submission_special_instructions 'No special instructions were received'