Synthesis, crystal structure and spectroscopic studies of a series of hexavanadate hybrids with multiple functional groups
Huang, Bo; Xiao, Zicheng; Wu, Baolin; Hu, Xiaokang; Hu, Xunliang; Wu, Pingfan; Wei, Yongge; Inorganic Chemistry Frontiers 4 (2017) 165–; doi:10.1039/C6QI00302H

data_4349532
_publ_section_title
;
 Synthesis, crystal structure and spectroscopic studies of a series of
 hexavanadate hybrids with multiple functional groups
;
_journal_issue                   1
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              165
_journal_paper_doi               10.1039/C6QI00302H
_journal_volume                  4
_journal_year                    2017
_chemical_formula_moiety         '2(C13 H13 O13.5 V3), 2(C16 H36 N)'
_chemical_formula_sum            'C58 H98 N2 O27 V6'
_chemical_formula_weight         1561.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-03-17
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_audit_update_record
;
2016-06-13 deposited with the CCDC.
2016-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 99.0881(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.3754(2)
_cell_length_b                   16.3585(3)
_cell_length_c                   18.4016(4)
_cell_measurement_reflns_used    5355
_cell_measurement_temperature    103.7
_cell_measurement_theta_max      29.2539
_cell_measurement_theta_min      2.9235
_cell_volume                     3381.27(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'A short history of SHELX (Sheldrick, 2007)/Bruker'
_diffrn_ambient_temperature      103.7
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   34.00   89.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9827   77.0000  120.0000 55

  2 omega  -26.00   17.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9827  -37.0000  -30.0000 43

  3 omega   52.00   90.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9827   52.0000  175.0000 38

  4 omega   -3.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9827   77.0000   90.0000 52

  5 omega   -5.00   63.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9827   77.0000  -30.0000 68
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0627220000
_diffrn_orient_matrix_UB_12      -0.0050281000
_diffrn_orient_matrix_UB_13      0.0055761000
_diffrn_orient_matrix_UB_21      0.0063408000
_diffrn_orient_matrix_UB_22      0.0340407000
_diffrn_orient_matrix_UB_23      0.0241828000
_diffrn_orient_matrix_UB_31      -0.0037628000
_diffrn_orient_matrix_UB_32      -0.0263745000
_diffrn_orient_matrix_UB_33      0.0301315000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15669
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.93
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.878
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         6633
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+5.6236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1213
_reflns_number_gt                5314
_reflns_number_total             6633
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00302h2.cif
_cod_data_source_block           exp_3913
_cod_database_code               4349532
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32