Structural and spectroscopic studies of a rare non-oxido V(v) complex crystallized from aqueous solution
Leggett, C. J.; Parker, B. F.; Teat, S. J.; Zhang, Z.; Dau, P. D.; Lukens, W. W.; Peterson, S. M.; Cardenas, A. J. P.; Warner, M. G.; Gibson, J. K.; Arnold, J.; Rao, L.; Chem. Sci. 7 (2016) 2775–; doi:10.1039/C5SC03958D

data_1542280
_publ_section_title
;
 Structural and spectroscopic studies of a rare non-oxido V(v) complex
 crystallized from aqueous solution
;
_journal_issue                   4
_journal_name_full               'Chem. Sci.'
_journal_page_first              2775
_journal_paper_doi               10.1039/C5SC03958D
_journal_volume                  7
_journal_year                    2016
_chemical_formula_sum            'C10 H16 N6 Na O6 V'
_chemical_formula_weight         390.22
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     'Intrinsic Phasing'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-07-17 deposited with the CCDC.
2016-01-14 downloaded from the CCDC.
;
_cell_angle_alpha                102.684(2)
_cell_angle_beta                 107.187(2)
_cell_angle_gamma                103.796(2)
_cell_formula_units_Z            2
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_cell_length_b                   8.7365(4)
_cell_length_c                   12.1972(5)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.25
_cell_measurement_theta_min      2.76
_cell_volume                     745.41(6)
_computing_cell_refinement       'Bruker SAINT v8.34a'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT v8.34a'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\w/\q shutterless scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13779
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         40.263
_diffrn_reflns_theta_min         2.756
_diffrn_source                   'Advanced Light Source station 11.3.1'
_exptl_absorpt_coefficient_mu    0.931
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/4 Bruker AXS Madison WI USA'
_exptl_crystal_colour            brown/orange
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_description       tablet
_exptl_crystal_F_000             400
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         7062
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+0.2437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0729
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6412
_reflns_number_total             7062
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03958d2.cif
_cod_data_source_block           cjl_2a_a
_cod_depositor_comments
'Adding full bibliography for 1542280--1542281.cif.'
_cod_original_cell_volume        745.41(5)
_cod_database_code               1542280
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.904
_shelx_estimated_absorpt_t_max   0.973
_shelx_res_checksum              30097
_shelx_hkl_checksum              85413