Coordination-Driven Self-Assembly of a 2D Graphite-Like Framework Constructed from High-Nuclear Ce10 Cluster Encapsulated Polyoxotungstates.
Ma, Pengtao; Wan, Rong; Wang, Yueyan; Hu, Feng; Zhang, Dongdi; Niu, Jingyang; Wang, Jingping; Inorganic chemistry 55 (2016) 918–924; doi:10.1021/acs.inorgchem.5b02473

data_4344531
_publ_section_title
;
 Coordination-Driven Self-Assembly of a 2D Graphite-Like Framework
 Constructed from High-Nuclear Ce10 Cluster Encapsulated
 Polyoxotungstates.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              918
_journal_page_last               924
_journal_paper_doi               10.1021/acs.inorgchem.5b02473
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'0.5(C2 Ce22 O418 P12 W96), 13(O), 6(C4 H12 N), C4 H10 N'
_chemical_formula_sum            'C29 H132 Ce11 N7 O222 P6 W48'
_chemical_formula_weight         14683.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-10-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.2062(10)
_cell_length_b                   31.0697(11)
_cell_length_c                   40.1622(14)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    296(2)
_cell_volume                     35196(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0971
_diffrn_reflns_av_unetI/netI     0.0719
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            178953
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.245
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.105
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1089 before and 0.0617 after correction.
The Ratio of minimum to maximum transmission is 0.6496.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.771
_exptl_crystal_description       block
_exptl_crystal_F_000             25644
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.22
_refine_diff_density_max         3.394
_refine_diff_density_min         -2.344
_refine_diff_density_rms         0.381
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         31600
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.0586
_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^)+(0.0576P)^2^+1702.9509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1670
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20526
_reflns_number_total             31600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02473_si_002.cif
_cod_data_source_block           1430500
_cod_database_code               4344531
_shelx_estimated_absorpt_t_max   0.117
_shelx_estimated_absorpt_t_min   0.056
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H) groups, All C(H,H,H) groups
2. Restrained distances
 N1-C2 = N1-C3 = N1-C4 = N1-C5
 1.47 with sigma of 0.01
 N2-C6 = N2-C7 = N2-C8 = N2-C9
 1.47 with sigma of 0.01
 N3-C10 = N3-C11 = N3-C12
 1.47 with sigma of 0.01
 N4-C13 = N4-C14 = N4-C15 = N4-C16
 1.47 with sigma of 0.01
 C2-C3 \\sim C2-C4 \\sim C2-C5 \\sim C3-C4 \\sim C3-C5 \\sim C4-C5
 with sigma of 0.02
 C6-C7 \\sim C6-C8 \\sim C6-C9 \\sim C7-C8 \\sim C7-C9 \\sim C8-C9
 with sigma of 0.02
 C13-C14 \\sim C13-C15 \\sim C13-C16 \\sim C14-C15 \\sim C14-C16 \\sim C15-C16
 with sigma of 0.02
3. Others
 Fixed Sof: H10B(0.5) H11B(0.5)
 Fixed Uiso: O6W(0.10872) O7W(0.11127) O8W(0.10652) C2(0.10903) C3(0.12281)
 C4(0.13099) C5(0.14171) C8(0.12346) C9(0.12601) C11(0.09871) C12(0.10845)
 C13(0.12967) C14(0.1247) C15(0.12915) C16(0.13478)
4.a Riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B)
4.b Me refined with riding coordinates:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,
 H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C12(H12A,H12B,
 H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,
 H16B,H16C)
;
_shelx_res_checksum              40297
_shelx_hkl_checksum              61803
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'