Mapping the formation areas of giant molybdenum blue clusters: a spectroscopic study.
Botar, Bogdan; Ellern, Arkady; Kögerler, Paul; Dalton transactions (Cambridge, England : 2003) 41 (2012) 8951–8959; doi:10.1039/c2dt30661a

data_7019594
_publ_section_title
;
 Mapping the formation areas of giant molybdenum blue clusters: a
 spectroscopic study.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8951
_journal_page_last               8959
_journal_paper_doi               10.1039/c2dt30661a
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'H432 K12 Mo102 Na2 O555 S14 V'
_chemical_formula_weight         20116.30
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug 2 2010,13:00:58)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.8199(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   44.4160(6)
_cell_length_b                   26.5633(3)
_cell_length_c                   44.7030(5)
_cell_measurement_reflns_used    99187
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5522
_cell_measurement_theta_min      2.8801
_cell_volume                     51215.4(11)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug 2 2010,13:00:58)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug 2 2010,13:00:58)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug 2 2010,13:00:58)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.4623
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            317408
_diffrn_reflns_theta_full        23.82
_diffrn_reflns_theta_max         23.82
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    2.708
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug 2 2010,13:00:58)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
;
_exptl_crystal_colour            dark-blue
_exptl_crystal_density_diffrn    2.708
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             38612
_exptl_crystal_size_max          0.3124
_exptl_crystal_size_mid          0.1693
_exptl_crystal_size_min          0.0636
_refine_diff_density_max         4.501
_refine_diff_density_min         -2.537
_refine_diff_density_rms         0.330
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3231
_refine_ls_number_reflns         39284
_refine_ls_number_restraints     696
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0851
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+8005.2617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2073
_refine_ls_wR_factor_ref         0.2251
_reflns_number_gt                32134
_reflns_number_total             39284
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30661a.txt
_cod_data_source_block           em3
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7019594