Facile synthesis of an organically-derivatized hexavanadate containing the remote amino group, TBA2[V6O13{(OCH2)3CNH2}2]
Bayaguud, Aruuhan; Chen, Kun; Wei, Yongge; CrystEngComm 18 (2016) 4042–; doi:10.1039/C5CE02534F

data_7224157
_publ_section_title
;
 Facile synthesis of an organically-derivatized hexavanadate containing
 the remote amino group, TBA2[V6O13{(OCH2)3CNH2}2]
;
_journal_issue                   22
_journal_name_full               CrystEngComm
_journal_page_first              4042
_journal_paper_doi               10.1039/C5CE02534F
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C24 H28 N2 O21 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C56 H100 N4 O21 V6'
_chemical_formula_weight         1471.04
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-12-16 deposited with the CCDC.
2016-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.47(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.598(2)
_cell_length_b                   19.518(4)
_cell_length_c                   15.301(3)
_cell_measurement_reflns_used    13908
_cell_measurement_temperature    153.1500
_cell_measurement_theta_max      31.5022
_cell_measurement_theta_min      2.0869
_cell_volume                     3462.5(12)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23314
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    0.847
_exptl_absorpt_correction_T_max  0.809
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bolck
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         6726
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0423P)^2^+2.0902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1040
_reflns_number_gt                6302
_reflns_number_total             6726
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce02534f2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 7224157--7224158.cif.'
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7224157