Low-valent vanadium catecholate clusters
Scales, Emma; Sorace, Lorenzo; Dei, Andrea; Caneschi, Andrea; Muryn, Christopher A.; Collison, David; McInnes, Eric J. L.; Chemical Science 1 (2010) 221–; doi:10.1039/c0sc00142b

data_1515764
_publ_section_title
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 Low-valent vanadium catecholate clusters
;
_journal_issue                   2
_journal_name_full               'Chemical Science'
_journal_page_first              221
_journal_paper_doi               10.1039/c0sc00142b
_journal_volume                  1
_journal_year                    2010
_chemical_formula_sum            'C67 H120 O24 V6'
_chemical_formula_weight         1615.27
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.59(3)
_cell_angle_beta                 74.53(3)
_cell_angle_gamma                82.69(3)
_cell_formula_units_Z            2
_cell_length_a                   13.520(3)
_cell_length_b                   18.220(4)
_cell_length_c                   19.290(4)
_cell_measurement_reflns_used    18496
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.226
_cell_measurement_theta_min      4.517
_cell_volume                     4540.6(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       'w\ rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS STATION 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.69420
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_sigmaI/netI    0.0851
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33491
_diffrn_reflns_theta_full        24.10
_diffrn_reflns_theta_max         24.10
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.648
_exptl_absorpt_correction_T_max  0.9808
_exptl_absorpt_correction_T_min  0.8293
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue/black
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1626
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.356
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     924
_refine_ls_number_reflns         15418
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0724
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1629P)^2^+2.2778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2100
_refine_ls_wR_factor_ref         0.2421
_reflns_number_gt                9869
_reflns_number_total             15418
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0sc00142b.txt
_cod_data_source_block           testp-1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'constrained' was replaced with
the value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        4540.6(16)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1515764