Assembly of Modular Asymmetric Organic-Inorganic Polyoxometalate Hybrids into Anisotropic Nanostructures
Mali H. Rosnes; Chiara Musumeci; Chullikkattil P. Pradeep; Jennifer S. Mathieson; De-Liang Long; Yu-Fei Song; Bruno Pignataro; Richard Cogdell; Leroy Cronin; Journal of the American Chemical Society 132 (2010) 15490–15492; doi:10.1021/ja1066338

data_4103455
_publ_section_title
;
 Assembly of Modular Asymmetric Organic-Inorganic Polyoxometalate Hybrids
 into Anisotropic Nanostructures
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15490
_journal_page_last               15492
_journal_paper_doi               10.1021/ja1066338
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety
'3(C16 H36 N +), (C26 H46 Mn Mo6 O24 3-), 2(C2 H3 N)'
_chemical_formula_sum            'C78 H160 Mn Mo6 N5 O24'
_chemical_formula_weight         2182.69
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.830(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.9788(3)
_cell_length_b                   16.1403(3)
_cell_length_c                   25.4293(3)
_cell_measurement_reflns_used    25346
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      67.5
_cell_measurement_theta_min      3.25
_cell_volume                     9697.3(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.44
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Oxford Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w & \p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            70117
_diffrn_reflns_theta_full        67.59
_diffrn_reflns_theta_max         67.59
_diffrn_reflns_theta_min         3.26
_diffrn_standards_decay_%        none
_diffrn_standards_number         71791
_exptl_absorpt_coefficient_mu    7.733
_exptl_absorpt_correction_T_max  0.540
_exptl_absorpt_correction_T_min  0.411
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4528
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.10
_refine_diff_density_min         -0.97
_refine_diff_density_rms         0.11
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     940
_refine_ls_number_reflns         17289
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+49.7577P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1406
_refine_ls_wR_factor_ref         0.1584
_reflns_number_gt                12237
_reflns_number_total             17289
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja1066338_si_002_2.cif
_cod_data_source_block           mr377b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        9697.3(2)
_cod_database_code               4103455