Solution-Phase Monitoring of the Structural Evolution of a Molybdenum Blue Nanoring
Haralampos N. Miras; Craig J. Richmond; De-Liang Long; Leroy Cronin; Journal of the American Chemical Society 134 (2012) 3816–3824; doi:10.1021/ja210206z

data_4117542
_publ_section_title
;
 Solution-Phase Monitoring of the Structural Evolution of a Molybdenum
 Blue Nanoring
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3816
_journal_page_last               3824
_journal_paper_doi               10.1021/ja210206z
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         '24(Na +), (H154 Mo186 O638 24-), 320(H2 O)'
_chemical_formula_sum            'H794 Mo186 Na24 O958'
_chemical_formula_weight         34524.95
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.979(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   29.4139(9)
_cell_length_b                   51.1644(9)
_cell_length_c                   30.5935(12)
_cell_measurement_reflns_used    9549
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      55.3
_cell_measurement_theta_min      3.38
_cell_volume                     41735(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.889
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_device_type  'Oxford Diffraction Gemini CCD'
_diffrn_measurement_method       '\w 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  0.0583
_diffrn_reflns_av_sigmaI/netI    0.1297
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            69631
_diffrn_reflns_theta_full        55.35
_diffrn_reflns_theta_max         55.35
_diffrn_reflns_theta_min         3.46
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    23.456
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.348
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
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            blue
_exptl_crystal_density_diffrn    2.747
_exptl_crystal_description       block
_exptl_crystal_F_000             33068
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.45
_refine_diff_density_min         -1.63
_refine_diff_density_rms         0.28
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1879
_refine_ls_number_reflns         23958
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.1132
_refine_ls_R_factor_gt           0.0757
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1193P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2068
_refine_ls_wR_factor_ref         0.2177
_reflns_number_gt                13529
_reflns_number_total             23958
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210206z_si_002.cif
_cod_data_source_block           hmfr5
_cod_original_cell_volume        41735(2)
_cod_database_code               4117542