Crystal structure of bis(3-(3-ethylureido)-N,N-dimethylpropan-1-aminium) bis (μ 3-2-(hydroxymethyl)-2-(oxidomethyl)propane-1,3-bis(olato))-(μ 6-oxo)-hexakis(μ 2-oxo)-hexaoxo-hexavanadium(V) – dichloromethane (1/1), C27H60Cl2N6O23V6
Hu, Xiaokang; Huang, Bo; Xiao, Zicheng; Wu, Pingfan; Zeitschrift für Kristallographie - New Crystal Structures 232 (2017) 849–850; doi:10.1515/ncrs-2017-0001

data_8106699
_publ_section_title
;
 Crystal structure of bis(3-(3-ethylureido)-N,N-dimethylpropan-1-aminium)
 bis (\m 3-2-(hydroxymethyl)-2-(oxidomethyl)propane-1,3-bis(olato))-(\m
 6-oxo)-hexakis(\m 2-oxo)-hexaoxo-hexavanadium(V) -- dichloromethane
 (1/1), C27H60Cl2N6O23V6
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              849
_journal_page_last               850
_journal_paper_doi               10.1515/ncrs-2017-0001
_journal_volume                  232
_journal_year                    2017
_chemical_formula_moiety
'2(C5 H9 O10.5 V3), 2(C8 H20 N3 O), 2(C0.5 H Cl)'
_chemical_formula_sum            'C27 H60 Cl2 N6 O23 V6'
_chemical_formula_weight         1213.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.932(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.1482(12)
_cell_length_b                   10.6096(4)
_cell_length_c                   17.4426(6)
_cell_measurement_reflns_used    3464
_cell_measurement_temperature    106.0
_cell_measurement_theta_max      29.2315
_cell_measurement_theta_min      3.0187
_cell_volume                     4838.3(3)
_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      106.0
_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  -65.00  -39.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.8148  131.0000 -134.0000 26

  2 omega  -50.00   42.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9711  -37.0000  -90.0000 92

  3 omega   34.00   70.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9711 -138.0000  159.0000 36

  4 omega  -42.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9711  -77.0000 -180.0000 91
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0267112000
_diffrn_orient_matrix_UB_12      -0.0093448000
_diffrn_orient_matrix_UB_13      -0.0049387000
_diffrn_orient_matrix_UB_21      -0.0047097000
_diffrn_orient_matrix_UB_22      0.0464054000
_diffrn_orient_matrix_UB_23      0.0282678000
_diffrn_orient_matrix_UB_31      -0.0006912000
_diffrn_orient_matrix_UB_32      0.0472123000
_diffrn_orient_matrix_UB_33      -0.0288096000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10699
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.02
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.304
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80951
_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            yellow
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.597
_refine_diff_density_min         -1.049
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         4756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0565
_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^)+(0.0605P)^2^+26.6512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1370
_refine_ls_wR_factor_ref         0.1477
_reflns_number_gt                3735
_reflns_number_total             4756
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2017-0001_suppl.cif
_cod_data_source_block           exp_1115
_cod_database_code               8106699
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32