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_7224158
_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         'C8 H18 N2 O19 V6, 4(H2 O)'
_chemical_formula_sum            'C8 H26 N2 O23 V6'
_chemical_formula_weight         823.95
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 104.20(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.381(2)
_cell_length_b                   12.311(3)
_cell_length_c                   9.6175(19)
_cell_measurement_reflns_used    8581
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.07
_cell_volume                     1191.6(5)
_computing_cell_refinement       'Rigaku RAPID AUTO Ver2.30'
_computing_data_collection       'Rigaku RAPID AUTO Ver2.30'
_computing_data_reduction        'Rigaku RAPID AUTO Ver2.30'
_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      296
_diffrn_detector_area_resol_mean '100x100 micron'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       Oscillation
_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  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5137
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    2.366
_exptl_absorpt_correction_T_max  0.492
_exptl_absorpt_correction_T_min  0.334
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         1230
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0285P)^2^+3.2886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0776
_reflns_number_gt                1152
_reflns_number_total             1230
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce02534f2.cif
_cod_data_source_block           c2m
_cod_depositor_comments
'Adding full bibliography for 7224157--7224158.cif.'
_cod_original_cell_volume        1191.6(4)
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7224158