Polyoxometalate precursors for precisely controlled synthesis of bimetallic sulfide heterostructure through nucleation-doping competition.
Tang, Yu-Jia; Zhang, A-Man; Zhu, Hong-Jing; Dong, Long-Zhang; Wang, Xiao-Li; Li, Shun-Li; Han, Min; Xu, Xiang-Xin; Lan, Ya-Qian; Nanoscale 10 (2018) 8404–8412; doi:10.1039/c8nr00925b

data_1549243
_publ_section_title
;
 Polyoxometalate precursors for precisely controlled synthesis of
 bimetallic sulfide heterostructure through nucleation-doping competition.
;
_journal_issue                   18
_journal_name_full               Nanoscale
_journal_page_first              8404
_journal_page_last               8412
_journal_paper_doi               10.1039/c8nr00925b
_journal_volume                  10
_journal_year                    2018
_chemical_formula_moiety         'Co Mo6 O24, 6(H2 O), 4(N)'
_chemical_formula_sum            'Co H12 Mo6 N4 O30'
_chemical_formula_weight         1182.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.143(17)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.403(14)
_cell_length_b                   10.995(13)
_cell_length_c                   11.715(14)
_cell_measurement_reflns_used    6387
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.430
_cell_measurement_theta_min      2.557
_cell_volume                     1446(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      296.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8790
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.814
_exptl_absorpt_coefficient_mu    3.191
_exptl_absorpt_correction_T_max  0.5633
_exptl_absorpt_correction_T_min  0.3307
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1185 before and 0.0739 after correction. The Ratio of minimum to maximum transmission is 0.5871. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.717
_exptl_crystal_description       plate
_exptl_crystal_F_000             1118
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.749
_refine_diff_density_min         -1.435
_refine_diff_density_rms         0.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3287
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0642
_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^)+(0.0483P)^2^+26.4396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1523
_refine_ls_wR_factor_ref         0.1641
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2668
_reflns_number_total             3287
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nr00925b1.cif
_cod_data_source_block           mo_como6_0m
_cod_depositor_comments          'Adding full bibliography for 1549243.cif.'
_cod_database_code               1549243
_shelx_shelxl_version_number     2016/4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O3W) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB)
;
_olex2_submission_special_instructions 'No special instructions were received'