Oxidation-driven self-assembly gives access to high-nuclearity molecular copper vanadium oxide clusters
Forster, Johannes; Rösner, Benedikt; Fink, Rainer H.; Nye, Leanne C.; Ivanovic-Burmazovic, Ivana; Kastner, Katharina; Tucher, Johannes; Streb, Carsten; Chemical Science 4 (2013) 418–; doi:10.1039/c2sc20942j

data_1514845
_publ_section_title
;
 Oxidation-driven self-assembly gives access to high-nuclearity molecular
 copper vanadium oxide clusters
;
_journal_issue                   1
_journal_name_full               'Chemical Science'
_journal_page_first              418
_journal_paper_doi               10.1039/c2sc20942j
_journal_volume                  4
_journal_year                    2013
_chemical_formula_moiety         '(C16 H36 N)4, (Cu6 V30 O86 N2), (C2 H3 N)6'
_chemical_formula_sum            'C76 H162 Cu6 N12 O88.66 V30'
_chemical_formula_weight         4561.64
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_hydrogens   notdet
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   20.411(3)
_cell_length_b                   20.411(3)
_cell_length_c                   40.340(5)
_cell_measurement_reflns_used    214
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.48
_cell_measurement_theta_min      6.12
_cell_volume                     14554(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            167266
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    2.084
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6348
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_platon_squeeze_details
;
;
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     839
_refine_ls_number_reflns         19763
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0751P)^2^+4.0292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1222
_reflns_number_gt                16489
_reflns_number_total             19763
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2sc20942j.txt
_cod_data_source_block           CS1029
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        14554(3)
_cod_original_sg_symbol_H-M      p_31_2_1
_cod_database_code               1514845